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Article(id=1276262865099165934, tenantId=1146029695717560320, journalId=1235980609244409860, issueId=1276262756814815737, articleNumber=null, orderNo=null, doi=10.3969/j.issn.1000-2561.2024.08.019, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1683216000000, receivedDateStr=2023-05-05, revisedDate=1688918400000, revisedDateStr=2023-07-10, acceptedDate=null, acceptedDateStr=null, onlineDate=1782214378856, onlineDateStr=2026-06-23, pubDate=1724515200000, pubDateStr=2024-08-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1782214378856, onlineIssueDateStr=2026-06-23, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1782214378856, creator=13701087609, updateTime=1782214378856, updator=13701087609, issue=Issue{id=1276262756814815737, tenantId=1146029695717560320, journalId=1235980609244409860, year='2024', volume='45', issue='8', pageStart='1521', pageEnd='1760', issueExtLink='null', onlineDate='null', pubDate='1724515200000', pubDateStr='2024-08-25', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1782214353040, creator='13701087609', updateTime=1782214460949, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1276263209816420382, tenantId=1146029695717560320, journalId=1235980609244409860, issueId=1276262756814815737, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1276263209816420383, tenantId=1146029695717560320, journalId=1235980609244409860, issueId=1276262756814815737, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=1696, endPage=1704, ext={EN=ArticleExt(id=1276262865338241264, articleId=1276262865099165934, tenantId=1146029695717560320, journalId=1235980609244409860, language=EN, title=Storage Properties of Yunyan 774 Concentrated Natural Latex, columnId=1236286112713470633, journalTitle=Chinese Journal of Tropical Crops, columnName=Post-harvest Treatment & Quality Safety, runingTitle=null, highlight=null, articleAbstract=

Yunyan 774 is a newly bred rubber tree cultivar in Yunnan, the research on its latex composition and properties is of great significance for its popularization and application. The changes of non-rubber components and colloidal properties, molecular weight and distribution of Yunyan 774 concentrated natural latex during storage, as well as the differences of crosslinking density, physical and mechanical properties, aging properties and latex particle size and distribution after 90 days of storage were measured and analyzed. The experimental results showed that the total solid content and ash content of Yunyan 774 remained unchanged after 90 days of storage, and the dry rubber content decreased by 1.1%, which was related to the reaction of some non-adhesive substances to form substances that could not be precipitated by adding acid. The content of volatile matter decreased slightly, but the content of acetone soluble content, water soluble content and nitrogen increased in different degrees. The content of advanced fatty acids of Yunyan 774 increased with the extension of storage time, and the ammonium soap with protective effect was generated, which played a role in improving the mechanical stability in the early stage. The thermal stability decreased gradually, and the viscosity decreased first and then was basically constant. The increase of volatile fatty acid content was not conducive to the preservation of latex. The physical mechanical properties and aging properties of Yunyan 774 latex vulcanized rubber film were better than those of the mixed strain. Compared with the mixed strain, the molecular weight distribution of Yunyan 774 was wider, the molecular weight was slightly lower, and the particle size was not different.

, authors=null, authorsList=Lihong WAN, Mingyuan YI, Lin FANG, Zhifen WANG, Jianhe LIAO, authorCompany=null, correspAuthors=Zhifen WANG, Jianhe LIAO, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1276262866785276162, articleId=1276262865099165934, tenantId=1146029695717560320, journalId=1235980609244409860, language=CN, title=新品系云研774浓缩天然胶乳贮存性能研究, columnId=1236286112877048492, journalTitle=热带作物学报, columnName=采后处理与质量安全, runingTitle=null, highlight=null, articleAbstract=

云研774作为云南新开割的橡胶品种，对其胶乳成分与性能的研究，以及对其推广应用具有重要意义。本研究以新品系云研774浓缩天然胶乳为对象，以混合品系为对照，研究云研774浓缩天然胶乳在贮存过程中非胶组分、胶体性能和分子量及其分布的变化，以及贮存90 d后胶乳硫化胶膜交联密度、物理机械性能、老化性能和胶乳粒子大小及其分布等。结果表明：贮存90 d后，云研774的总固体含量和灰分含量基本不变，干胶含量下降1.1%，这与一些非胶物质反应生成加酸无法沉淀的物质有关；挥发物含量略有下降，而丙酮溶物含量、水溶物和氮含量则有不同程度的增加。云研774的高级脂肪酸含量随着贮存时间的延长而增加，生成有保护作用的铵皂，在前期起到提高机械稳定性的作用；热稳定度则逐渐下降，黏度先降低后基本恒定。挥发脂肪酸含量的增加在一定程度上不利于胶乳的保存；云研774胶乳硫化胶膜的物理机械性能和老化性能优于混合品系，与混合品系相比，云研774的分子量分布变宽，分子量稍低，粒径大小相差不大。

, authors=

万立红（1995—），女，硕士研究生，研究方向：天然橡胶基础与改性。

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* 汪志芬（WANG Zhifen），E-mail：
廖建和（LIAO Jianhe），E-mail：。
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万立红（1995—），女，硕士研究生，研究方向：天然橡胶基础与改性。

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万立红（1995—），女，硕士研究生，研究方向：天然橡胶基础与改性。

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Polymers, 2022, 14(9): 1759., articleTitle=Influence of non-rubber components on the properties of unvulcanized natural rubber from different clones, refAbstract=null)], funds=[Fund(id=1276269141120127645, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, awardId=2020B020217001, language=CN, fundingSource=广东省重点领域研发计划项目(2020B020217001), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1276269127106957922, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, xref=null, ext=[AuthorCompanyExt(id=1276269127119540835, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, companyId=1276269127106957922, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=College of Materials Science and Engineering, Hainan University, Haikou, Hainan 570228, China), AuthorCompanyExt(id=1276269127132123748, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, companyId=1276269127106957922, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=海南大学材料科学与工程学院，海南海口　570228)])], figs=[ArticleFig(id=1276269136825160329, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=EN, label=Fig. 1, caption=Changes in total solid content, dry rubber content and non-colloidal compoent of concentrated natural rubber latex during storage, figureFileSmall=1BcQpZ6UVsn+OkzkSx2HMw==, figureFileBig=m86arYw4UDKe7ZoxfzsYXQ==, tableContent=null), ArticleFig(id=1276269136892269194, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=CN, label=图1, caption=贮存过程中浓缩天然胶乳总固体含量、干胶含量和非胶含量的变化, figureFileSmall=1BcQpZ6UVsn+OkzkSx2HMw==, figureFileBig=m86arYw4UDKe7ZoxfzsYXQ==, tableContent=null), ArticleFig(id=1276269137278145163, 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journalId=1235980609244409860, articleId=1276262865099165934, language=CN, label=图6, caption=混合品系和云研774贮存前后浓缩天然胶乳分子量分布曲线, figureFileSmall=Odo+QJIOeul/CV6prIfUtg==, figureFileBig=ampiqeoOMDZO7Grh2ph2fw==, tableContent=null), ArticleFig(id=1276269140214157973, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=EN, label=Fig. 7, caption=Physical and mechanical properties of mixed strain and Yunyan 774 concentrated natural latex, figureFileSmall=gcV8qU0NthcxWqumcI/FSA==, figureFileBig=GVcJ9wpA+fRbON8tAC6Pgw==, tableContent=null), ArticleFig(id=1276269140289655446, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=CN, label=图7, caption=混合品系和云研774浓缩天然胶乳硫化胶膜的物理机械性能, figureFileSmall=gcV8qU0NthcxWqumcI/FSA==, figureFileBig=GVcJ9wpA+fRbON8tAC6Pgw==, tableContent=null), ArticleFig(id=1276269140360958615, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=EN, label=Tab. 1, caption=

Latex vulcanization list (dry basis ratio)

, figureFileSmall=null, figureFileBig=null, tableContent=
原料Material用量（质量份）Dosage (mass)
浓缩天然胶乳100
氢氧化钾（20%）0.30
硫磺（50%）0.75
促进剂ZDC（40%）0.75
氧化锌（40%）0.40
纯水适量
), ArticleFig(id=1276269140428067480, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=CN, label=表1, caption=

胶乳硫化配方（干基配比）

, figureFileSmall=null, figureFileBig=null, tableContent=
原料Material用量（质量份）Dosage (mass)
浓缩天然胶乳100
氢氧化钾（20%）0.30
硫磺（50%）0.75
促进剂ZDC（40%）0.75
氧化锌（40%）0.40
纯水适量
), ArticleFig(id=1276269140591645337, tenantId=1146029695717560320, journalId=1235980609244409860, articleId=1276262865099165934, language=EN, label=Tab. 2, caption=

Molecular weight and distribution of concentrated natural latex

, figureFileSmall=null, figureFileBig=null, tableContent=
贮存时间Storage time/d样品Sample数均分子量Mn/10–5重均分子量Mw/10–5Z均分子量Mz/10–5宽度系数Mw/Mn分散系数Mz/Mw
0混合品系9.1310.4411.741.141.29
云研7746.998.569.941.221.17
90混合品系8.279.4010.511.141.12
云研7746.318.1710.131.311.29
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浓缩天然胶乳分子量及其分布

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贮存时间Storage time/d样品Sample数均分子量Mn/10–5重均分子量Mw/10–5Z均分子量Mz/10–5宽度系数Mw/Mn分散系数Mz/Mw
0混合品系9.1310.4411.741.141.29
云研7746.998.569.941.221.17
90混合品系8.279.4010.511.141.12
云研7746.318.1710.131.311.29
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Mechanical properties of mixed strain and Yunyan 774 concentrated natural latex

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样品Sample拉伸强度Tensile strength/MPa300%定伸应力Stress at 300% elongation/MPa500%定伸应力Stress at 500% elongation/MPa断裂伸长率Elongation at break/%
混合品系28.260.400.82913
云研77430.070.350.711080
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混合品系和云研774浓缩天然胶乳的力学性能

, figureFileSmall=null, figureFileBig=null, tableContent=
样品Sample拉伸强度Tensile strength/MPa300%定伸应力Stress at 300% elongation/MPa500%定伸应力Stress at 500% elongation/MPa断裂伸长率Elongation at break/%
混合品系28.260.400.82913
云研77430.070.350.711080
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新品系云研774浓缩天然胶乳贮存性能研究
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万立红 , 仪明源 , 方林 , 汪志芬 * , 廖建和 *
热带作物学报 | 采后处理与质量安全 2024,45(8): 1696-1704
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热带作物学报 |采后处理与质量安全 2024 , 45 (8) : 1696 -1704
新品系云研774浓缩天然胶乳贮存性能研究
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万立红（1995—），女，硕士研究生，研究方向：天然橡胶基础与改性。

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万立红, 仪明源, 方林, 汪志芬* , 廖建和*
作者信息
  • 海南大学材料科学与工程学院，海南海口　570228
通讯作者:
* 汪志芬（WANG Zhifen），E-mail：
廖建和（LIAO Jianhe），E-mail：。
Storage Properties of Yunyan 774 Concentrated Natural Latex
Lihong WAN, Mingyuan YI, Lin FANG, Zhifen WANG* , Jianhe LIAO*
Affiliations
  • College of Materials Science and Engineering, Hainan University, Haikou, Hainan 570228, China
出版时间: 2024-08-25 doi: 10.3969/j.issn.1000-2561.2024.08.019
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摘要
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云研774作为云南新开割的橡胶品种，对其胶乳成分与性能的研究，以及对其推广应用具有重要意义。本研究以新品系云研774浓缩天然胶乳为对象，以混合品系为对照，研究云研774浓缩天然胶乳在贮存过程中非胶组分、胶体性能和分子量及其分布的变化，以及贮存90 d后胶乳硫化胶膜交联密度、物理机械性能、老化性能和胶乳粒子大小及其分布等。结果表明：贮存90 d后，云研774的总固体含量和灰分含量基本不变，干胶含量下降1.1%，这与一些非胶物质反应生成加酸无法沉淀的物质有关；挥发物含量略有下降，而丙酮溶物含量、水溶物和氮含量则有不同程度的增加。云研774的高级脂肪酸含量随着贮存时间的延长而增加，生成有保护作用的铵皂，在前期起到提高机械稳定性的作用；热稳定度则逐渐下降，黏度先降低后基本恒定。挥发脂肪酸含量的增加在一定程度上不利于胶乳的保存；云研774胶乳硫化胶膜的物理机械性能和老化性能优于混合品系，与混合品系相比，云研774的分子量分布变宽，分子量稍低，粒径大小相差不大。

浓缩天然胶乳  /  云研774  /  非胶组分  /  胶体性能  /  力学性能

Yunyan 774 is a newly bred rubber tree cultivar in Yunnan, the research on its latex composition and properties is of great significance for its popularization and application. The changes of non-rubber components and colloidal properties, molecular weight and distribution of Yunyan 774 concentrated natural latex during storage, as well as the differences of crosslinking density, physical and mechanical properties, aging properties and latex particle size and distribution after 90 days of storage were measured and analyzed. The experimental results showed that the total solid content and ash content of Yunyan 774 remained unchanged after 90 days of storage, and the dry rubber content decreased by 1.1%, which was related to the reaction of some non-adhesive substances to form substances that could not be precipitated by adding acid. The content of volatile matter decreased slightly, but the content of acetone soluble content, water soluble content and nitrogen increased in different degrees. The content of advanced fatty acids of Yunyan 774 increased with the extension of storage time, and the ammonium soap with protective effect was generated, which played a role in improving the mechanical stability in the early stage. The thermal stability decreased gradually, and the viscosity decreased first and then was basically constant. The increase of volatile fatty acid content was not conducive to the preservation of latex. The physical mechanical properties and aging properties of Yunyan 774 latex vulcanized rubber film were better than those of the mixed strain. Compared with the mixed strain, the molecular weight distribution of Yunyan 774 was wider, the molecular weight was slightly lower, and the particle size was not different.

concentrated natural latex  /  Yunyan 774  /  non-colloidal component  /  colloidal properties  /  mechanical property
万立红, 仪明源, 方林, 汪志芬, 廖建和. 新品系云研774浓缩天然胶乳贮存性能研究. 热带作物学报, 2024 , 45 (8) : 1696 -1704 . DOI: 10.3969/j.issn.1000-2561.2024.08.019
Lihong WAN, Mingyuan YI, Lin FANG, Zhifen WANG, Jianhe LIAO. Storage Properties of Yunyan 774 Concentrated Natural Latex[J]. Chinese Journal of Tropical Crops, 2024 , 45 (8) : 1696 -1704 . DOI: 10.3969/j.issn.1000-2561.2024.08.019
正文
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天然胶乳是从产胶植物中提取的一种天然高分子材料[1-3]，因其良好的综合性能，广泛应用于日常生活、医疗卫生以及国防科技等领域。天然胶乳良好的综合性能主要来源于其独特的分子结构与非胶组分[4]。由于天然胶乳是一种生物合成的高聚物，其产地和品系等因素均会对浓缩天然胶乳的组成与性能产生影响[5]，不同品系的天然胶乳，其化学成分不同，即使是在相同工艺条件下，所制备的浓缩天然胶乳性质也有所不同。此外，在投入生产加工前，浓缩天然胶乳通常会根据不同胶乳制品的生产工艺和配方，将浓缩天然胶乳贮存一段时间以达到胶乳制品对胶乳胶体性能和非胶组分等因素的要求[6-8]。天然浓缩胶乳在贮存过程中，其非胶组分会发生变化，不同品系的浓缩天然胶乳的组成与性能不同，贮存过程中的性能变化也是不一样的。
云研774是云南新开割的橡胶品系，有关该品系浓缩天然胶乳的组成、性能以及贮存性能的研究，尚无报道。本研究以云研774制备的浓缩天然胶乳为对象，以混合品系作对照，研究贮存90 d内云研774浓缩天然胶乳的主要非胶组分、胶体性能等的变化趋势，考察贮存90 d后浓缩天然胶乳的粒子形态结构、硫化胶膜的物理机械性能和老化性能，以及贮存前后浓缩天然胶乳的分子量及其分布状况。研究结果可为新品系云研774浓缩天然胶乳制备胶乳制品提供理论指导。
1　材料与方法
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1.1　材料
1.1.1　主要材料与试剂
混合品系（云南当地PB86、PR107、PPIM60以及云研774品种的混合）和云研774新鲜胶乳由西双版纳云锰新兴天然橡胶有限公司提供。丙酮、三氯甲烷、氨水、五水合硫酸铜、氯化铵均由西陇科学股份有限公司提供。氧化锌（ZnO）、硫磺（S）、二乙基二硫代氨基甲酸锌（ZDC）、氢氧化钾（KOH）均为分析纯。
1.1.2　主要仪器
KDN全自动凯氏定氮仪，浙江托普云农科技股份有限公司；H1650型离心机，湖南湘仪实验室仪器公司；UV-1200型紫外分光光度计，翱翔仪器（上海）有限公司；AL-7000-SV2型，高铁科技股份有限公司；ZetasizernanoZS90激光粒度分析仪，Malvern Instrument；滚动落球黏度计，FUNGILAB；旋转黏度计，上海昌吉地质仪器有限公司；Dunlop-Klaxon胶乳机械稳定度测定仪，英国KLAXON公司；Waters 515凝胶色谱仪，美国Waters公司；BHO-401A老化试验箱，上海一恒科学仪器有限公司；MDR- 2000E型无转子硫化仪，无锡鑫园电子化工设备厂。
1.2　方法
1.2.1　浓缩天然胶乳的制备
于新鲜胶乳中，加氨量为0.68%，加皂量为万分之三，然后用离心机进行离心处理，得到混合品系和云研774两种浓缩天然胶乳，并在常温下密闭贮存。
1.2.2　浓缩天然胶乳胶膜的制备
将混合品系和云研774胶乳过滤后，倒入平板玻璃上自然晾干成胶膜，装入保鲜袋中密封，放入干燥器中，备用。
1.2.3　浓缩天然胶乳硫化胶膜的制备
按照表1将各种配合剂和适量纯水加入浓缩天然胶乳中，60 ℃硫化0.5 h，降温、过滤，倒入水平玻璃板上自然晾干成膜，再放入100℃烘箱硫化1.5 h。
1.2.4　项目测试
（1）浓缩天然胶乳总固体含量（TSC）和干胶含量（DRC）。按照GB/T 8298—2017和GB/T 8299—2008测定总固体含量和干胶含量。
（2）浓缩天然胶乳非胶组分。按照GB/T 4498—1997测定灰分含量；按照NY/T 1527—2007测定水溶物含量；按照GB/T 249131—2009测定挥发物含量；按照GB/T 8808—2008测定丙酮溶物含量；按照GB/T 8088—1999测定氮含量。
（3）浓缩天然胶乳挥发脂肪酸值（VFANO）。按照GB/T 8292—2008测定挥发脂肪酸值。
（4）浓缩天然胶乳高级脂肪酸。称取6 g浓缩天然胶乳置于烧杯中，调节总固体含量，加入三氯甲烷和无水乙醇混合试剂（2∶1，V/V），通过搅拌过滤、反复挤压、水浴蒸干、酸化残渣，将酸化液抽提，在酚酞指示剂下，用KOH标准溶液滴定溶液至出现持久（30 s）的淡红色，按以下公式计算高级脂肪酸含量（HL）：
式中，N为KOH标准溶液当量浓度；V为滴定样品消耗KOH体积（mL）；V0为滴定空白消耗KOH体积（mL）；E为油酸克当量（282.47 g）；W为胶乳样品量（g）。
（5）浓缩天然胶乳胶体性能。按照GB/T 8301—2008测定胶乳机械稳定度；按照GB/T 14792.2—2008测定胶乳黏度。
（6）热稳定度测定。称取50 g浓缩天然胶乳，调节胶乳氨含量和总固体含量，通恒温水至70℃后，称取处理后胶乳12 g，快速加入3 mL锌氨络离子，倒入转筒，开始计时，黏度计指针摆动至规定值60格时所需时间即为热稳定度。
（7）激光粒度仪测试。取一滴浓缩天然胶乳于1 L水中，稀释至原浓度0.02%左右，采用Zatasizer nano ZS900激光粒度仪测试浓缩天然胶乳粒径及其粒径分布。
（8）凝胶渗透色谱测试[9]。将天然胶乳胶膜样品浸泡于色谱纯四氢呋喃溶液中，浓度为3 mg/L，避光保存至胶乳完全溶解。流动相为四氢呋喃，用Waters 515型凝胶色谱仪测定天然胶乳分子量及其分布状况。
（9）硫化胶膜物理机械性能测试。分别按照GB/T 528—2009和GB/T 529—2009测定硫化胶膜的拉伸强度和撕裂强度。
（10）交联密度测试。采用平衡溶胀法，根据Flory-Rehner方程[10]计算交联密度。
（11）热氧老化试验。按照国家标准GB/T 3512—2014进行热氧老化试验。
2　结果与分析
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2.1　贮存过程中浓缩天然胶乳总固体含量和干胶含量的变化
混合品系和云研744浓缩天然胶乳贮存90 d内的总固体含量、干胶含量及非胶组分变化趋势见图1。如图1所示，随着贮存时间的延长，混合品系和云研774浓缩天然胶乳的总固体含量基本保持不变，而干胶含量逐渐减少，非胶组分含量整体呈上升趋势。这主要是由于氨与胶乳中某些非胶组分发生反应，使原先可以通过加酸沉淀出来的物质，生成加酸无法沉淀的物质。在贮存早期，因参与这种反应的物质较多，浓度大，因此在初期干胶含量下降幅度较大[11]，经过贮存90 d后，混合品系的干胶含量下降0.29%，云研774的干胶含量下降1.10%。由此看出，云研774胶乳中加酸沉淀出的非胶组分多于混合品系。
2.2　贮存过程中浓缩天然胶乳主要非胶组分的变化
非胶组分作为胶乳中的重要组成成分，影响橡胶分子的结构与性能。因此，有必要探究浓缩天然胶乳贮存期间主要非胶组分的变化趋势。灰分含量在一定程度上表征了胶乳样品的金属盐含量。如图2A所示，贮存90 d后，云研774和混合品系胶乳的灰分含量相差不大，且符合国家标准。混合品系和云研774浓缩天然胶乳挥发物含量随贮存时间的变化见图2B，90 d后，云研774胶乳的挥发物含量小于1%，符合国家标准，而混合品系胶乳的挥发物含量稍高。影响胶乳挥发物含量的因素有很多，如蛋白质含量、水溶物含量或氨含量，以及胶乳贮存时的空气湿度均对胶乳挥发物含量有很大影响。
如图2C和图2D所示，随着贮存时间的延长，混合品系和云研774胶乳的水溶物含量和丙酮溶物含量整体均呈上升趋势，且贮存90 d后，云研774胶乳的水溶物含量低于混合品系。其原因在于贮存后期混合品系胶粒表面的蛋白质水解生成溶于水的氨基酸多于云研774胶乳。影响丙酮溶物含量的因素有很多，如磷脂一般不溶于丙酮，而加氨保存后，磷脂水解生成硬脂酸、油酸等溶于丙酮的长链脂肪酸。
混合品系和云研774浓缩天然胶乳氮含量随贮存时间的变化见图2E。经过贮存90 d，混合品系浓缩天然胶乳的氮含量由最初的0.29%降低至0.19%，而云研774胶乳的氮含量由0.25%升至0.29%。这与胶乳自身的蛋白质含量有关，以及贮存过程中构成胶乳保护层的蛋白质在氨存在下发生的水解反应有关。同时，除分布在胶粒表面的蛋白质外，其余大部分乳清相和底部黄色体的游离蛋白质分布状况也与蛋白质的变化情况密切相关。
2.3　贮存过程中浓缩天然胶乳挥发脂肪酸值和高级脂肪酸含量的变化
如图3所示，贮存90 d后，混合品系和云研774浓缩天然胶乳的挥发脂肪酸值（VFANO）和高级脂肪酸（HL）含量均呈上升趋势。贮存过程中胶乳的水溶物含量增加，为胶乳中的细菌提供更为丰富的碳水化合物，从而产生更多的挥发脂肪酸。贮存90 d后，混合品系和云研774胶乳高级脂肪酸含量的增长率分别为24.6%和21.0%。在胶乳贮存过程中高级脂肪酸含量增加的原因有以下两方面：类脂物水解释放高级脂肪酸；胶乳丙酮溶物中本身也含有一定的高级脂肪酸。因此，贮存期间高级脂肪酸含量随贮存时间的变化趋势与胶乳本身的丙酮溶物含量的变化趋势存在相关性。
2.4　贮存过程中混合品系和云研774浓缩天然胶乳胶体性能的变化
如图4A所示，随着贮存时间的延长，混合品系和云研774浓缩天然胶乳的机械稳定度均呈先上升后下降的趋势。这与贮存期间胶粒保护层上起稳定作用的蛋白质和类脂物的水解速率有关。在贮存前期，胶乳中起稳定作用的高级脂肪酸皂的产生速率明显快于蛋白质的水解速率[8,11]，因此，混合品系和云研774浓缩天然胶乳的机械稳定度在贮存30 d内均明显升高，但在贮存30 d后，挥发脂肪酸的生成导致体系中的氢离子浓度上升，胶乳稳定性降低，因此贮存后期机械稳定度出现一定程度的下降。贮存90 d时，云研774胶乳的机械稳定度比混合品系低390 s。贮存90 d后，2种浓缩天然胶乳的机械稳定度均达到出厂标准。
热稳定性是指胶乳温度升高时对其凝固具有的抵抗能力，对于衡量胶乳胶凝及成膜性能具有重要意义。如图4B所示。刚离心的云研774胶乳的热稳定度为86 s，低于混合品系的热稳定度。经过贮存60 d后，混合品系和云研774浓缩天然胶乳的热稳定度均明显下降，混合品系的热稳定度为95 s，云研774的热稳定度为18 s。贮存后期挥发脂肪酸含量增加导致氧化锌在胶乳中溶解度增加，锌氨络离子生成量增加。这些锌氨络离子一部分用于中和胶粒阴电荷，另一部分与保护层反应生成不溶性铵皂或铵盐，进而降低浓缩天然胶乳的热稳定度。
胶乳停放过程中黏度的变化对胶乳制品工艺具有重要的参考意义，黏度过高，胶乳工艺处理时，耗能增加，且容易存在制品表面成型不均匀或形成气泡等问题。贮存过程中混合品系和云研774浓缩天然胶乳黏度的变化见图4C。刚经过离心处理的混合品系胶乳的黏度为27.3 mPa·s，云研774的黏度为29.7 mPa·s，经过存放90 d后，混合品系和云研774胶乳的黏度分别下降至11.9 mPa·s和11.4 mPa·s。胶乳黏度与其胶乳本身某些非胶组分水解有关，在贮存一段时间后，胶乳中的磷脂水解生成高级脂肪酸等表面活性物质，使胶乳的黏度快速下降，当这类物质释放完全后，胶乳的黏度便趋于稳定。
2.5　浓缩天然胶乳粒径分析
图5是混合品系和云研774浓缩天然胶乳粒径分布图。由图5可知，与混合品系相比，云研774胶乳的粒径分布范围较窄，但粒径分布强度较强。混合品系和云研774胶乳的平均粒径相差不大，分别为433.0、445.9 mm，分散度指数（PDI）分别为0.276和0.209。胶乳的组分、结构以及性质很大程度上取决于橡胶树本身，因此，胶乳的粒径分布与品系密切相关。此外，胶乳粒径分布可能与胶乳不溶性铵皂的生成也有关。贮存期内，氧化锌与胶乳保护层反应生成不溶性铵皂，胶粒相互聚集，表现为部分胶乳粒子的粒径偏大，这与胶乳贮存过程中的热稳定度下降结果一致。
2.6　浓缩天然胶乳分子量分析
表2和图6是贮存前后混合品系和云研774浓缩天然胶乳的分子量（M）及其分布状况。结果表明，云研774胶乳的数均分子量（Mn）、重均分子量（Mw）、Z均分子量（Mz）均低于混合品系。就分子量分布情况而言，云研774胶乳的分子量分布较广，这与胶乳自身的生理特性有关。贮存90 d后，混合品系的Mn、Mw和Mz分别比贮存前降低0.86×105、1.04×105和1.23×105，云研774的Mn和Mw较贮存前降低0.68×105、0.39×105，而Mz则比贮存前增加0.19×105。混合品系的Mw/Mn贮存后稍有下降，而云研774的Mw/Mn则明显增加。这些结果均表明贮存过程中混合品系和云研774浓缩天然胶乳的分子量及其分布会发生不同程度的变化。
2.7　混合品系和云研774浓缩天然胶乳硫化胶膜物理机械性能分析
浓缩天然胶乳硫化胶膜物理机械性能是衡量胶乳制品尤其是浸渍制品产品性能的重要指标。通过测定混合品系和云研774硫化胶膜的物理机械性能可知，混合品系硫化胶膜的拉伸强度为28.26 MPa，云研774的拉伸强度为30.07 MPa（图7A，表3）。混合品系的撕裂强度为60.13 kN/m，云研774的撕裂强度为34.56 kN/m（图7B）。硫化胶膜的物理机械性能与其非橡胶组分尤其是蛋白质与磷脂的含量有关，蛋白质和磷脂与NR链的端基相互作用，形成端相连网络[12-14]，这种自然存在的网络，能够将瞬时缠结转化为永久缠结，进一步作为有效交联点[15]。当受到定向作用时，则更多的能量被消耗用于橡胶分子链的移动，从而获得更高的物理机械性能。如图7C所示，混合品系硫化胶膜的交联密度低于云研774硫化胶膜。与上述分析一致。
如图7D所示，经过48 h热氧老化后混合品系的拉伸强度保持率为40.0%，云研774的拉伸强度保持率为49.0%，表明云研774的耐老化性能优于混合品系。有研究表明，胶乳中的蛋白质和丙酮溶物具有抗氧化作用的物质，可以延缓胶乳制品老化，进而影响胶乳制品的使用寿命[16]。
3　讨论
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本研究以云南新培育的橡胶品种云研774为研究对象，通过与市面上传统的混合品系相比，分析云研774浓缩天然胶乳贮存后的总固体含量、干胶含量、非胶组分、胶体性能和分子量大小及其分布的变化情况，研究贮存90 d后云研774的硫化胶膜的物理机械性能、老化性能以及胶乳粒子粒径及其分布状况。
结果发现，就橡胶中的总固体含量和干胶含量而言，云研774高于混合品系。除挥发物、丙酮溶物和氮含量外，云研774浓缩天然胶乳的其他非胶组分与混合品系相差不大。与混合品系相比，云研774浓缩天然胶乳的挥发物含量和丙酮溶物含量分别下降0.23%和0.69%，氮含量则增加0.10%。与混合品系相比，云研774浓缩天然胶乳的机械稳定度、热稳定度均低于混合品系，黏度则相差不大。云研774的拉伸强度和撕裂强度分别为30.07 MPa和34.56 kN/m，老化48 h后，云研774的应力保持率为49.0%，力学性能和老化性能均优于混合品系。说明云研774的有效交联点多于混合品系。同时，云研774的分子量分布更为广泛但分子量稍低，而粒径大小相差不大。
同时，随着贮存时间的延长，混合品系和云研774浓缩天然胶乳的总固体含量和灰分含量基本不变，干胶含量逐渐减少。云研774浓缩天然胶乳的丙酮溶物含量、水溶物含量和氮含量均有不同幅度的增加，混合品系的挥发物含量、丙酮溶物含量和水溶物含量同样也有不同幅度的增加，这与贮存期间一些非胶物质在加氨胶乳中发生的化学反应有关。经过贮存90 d后，混合品系和云研774的挥发脂肪酸含量增加，这与细菌利用胶乳体系中的水溶物有关。同时混合品系和云研774的高级脂肪酸含量分别增加24.6%和21.0%。说明加氨胶乳中，丙酮溶物中的高级脂肪酸生成的铵皂，可在胶粒表面起到稳定作用。而机械稳定度、黏度和热稳定度在贮存后期均有明显下降，这为胶乳制品原料停放过程中胶体性能的变化趋势提供参考。本研究结果表明，贮存90 d后，混合品系和云研774的分子量均有一定程度的下降，但云研774的分子量分布范围更广泛。
此前，NUN-ANAN等[5]开展了巴西橡胶树不同无性系（RRIM600、PB235和RRTI408）性状的研究，揭示不同品系胶乳非胶组分对天然胶乳各项性能的影响。LEHMAN等[17]以RRIM600、RRIT251、PB235和BPM24混合品系和云研774巴西橡胶树为研究对象，研究了混合品系和云研774新鲜天然胶乳和浓缩天然胶乳对非胶组分相关性能的影响，研究发现，混合品系和云研774浓缩天然乳胶的蛋白质含量、表面张力和颜色均低于新鲜天然乳胶。但浓缩天然胶乳的总固体含量、干胶含量、黏度和粒径均高于新鲜天然乳胶。SAIWARI等[2]研究了RRIT251、PB235和RRIM600三个天然橡胶无性系的胶乳结构与硫化性能之间的关系，结果表明，影响混合品系和云研774硫化胶力学性能的关键因素均在于橡胶本身分子量及其分布状况。这是因为较高的平均分子量为交联反应提供了更大的活性位点，而蛋白质含量决定了未硫化橡胶中凝胶的形成。
云研774作为一种云南新开割的天然橡胶品系，对其新鲜胶乳和浓缩天然胶乳的生理参数及结构与性能的研究尚无报道。而现阶段国内外学者缺乏对混合品系和云研774浓缩天然胶乳从生产到投入使用过程中，贮存90 d内浓缩天然胶乳的主要非胶组分、胶体性能等应用性质变化趋势，硫化胶膜物理机械性能以及胶乳粒子形态结构的研究。因此，本研究结果为探究云研774胶乳各组分与性能之间的内在联系，为云研774应用于胶乳制品提供可靠的理论指导。
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  • 广东省重点领域研发计划项目(2020B020217001)
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2024年第45卷第8期
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doi: 10.3969/j.issn.1000-2561.2024.08.019
  • 接收时间：2023-05-05
  • 首发时间：2026-06-23
  • 出版时间：2024-08-25
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  • 收稿日期：2023-05-05
  • 修回日期：2023-07-10
基金
广东省重点领域研发计划项目(2020B020217001)
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    海南大学材料科学与工程学院，海南海口　570228

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* 汪志芬（WANG Zhifen），E-mail：
廖建和（LIAO Jianhe），E-mail：。
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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