有机硅丙烯酸酯增深剂的制备及应用

由乙烯基三乙氧基硅烷与KH-550、丙烯酸酯类单体在阴/非离子表面活性剂存在下，通过乳液聚合制得带蓝光的半透明有机硅丙烯酸酯乳液．该乳液粘度小，有机硅质量分数15％，总固体质量分数30％，该增深剂既可单独使用，也可与氨基硅油乳液复配，经蓝色16电力纺、黑色03双绉等真丝产品增深，其增深度可达15％，但亲水性有所下降．     

核壳型氟硅无皂拒水剂的合成及其拒水性能

为获得具有优良拒水性能的拒水剂,以甲基丙烯酸甲酯(MMA)、甲基丙烯酸月桂酯(LMA)、甲基丙烯酸十二氟庚酯(G-04)和乙烯基三乙氧基硅烷(KH-151)为反应单体,采用核壳乳液聚合法,合成核壳型氟硅无皂拒水剂.结果表明,当可聚合乳化剂(DNS-86:DNS-1035=2:1)质量分数为1.5%,壳层功能单体(G-04:KH-151=6∶1)质量占壳单体总质量的70%,引发剂质量分数为1%,交联单体质量分数1%时,合成的乳液性能稳定,且用其整理后的棉织物对水的接触角可达到144.6°,静水压达到2.32kPa,喷淋等级为4级.     

低温交联型聚丙烯酸酯涂层剂的合成及应用

以丙烯酸酯(BA和MMA)、丙烯酸(AA)、双丙酮丙烯酰胺(DAAM)等为主要原料,合成水性聚丙烯酸酯;中和后,添加交联剂己二酸二酰肼(ADH),合成了低温交联型聚丙烯酸酯涂层剂。通过单因素分析试验,优化涂层剂的合成工艺条件:乳化剂5%,引发剂0.6%,DAAM 6%(均为占单体总质量的百分比),摩尔分数比n(DAAM)∶n(ADH)=1∶1。在焙烘温度为130℃和焙烘时间为3 min的条件下,涤纶织物经该涂层剂整理后的湿摩擦牢度可达3~4级,干摩擦色牢度可达4级,皂洗色牢度可达4~5级,耐静水压为3.25 kPa,透湿量为1 105.38 g/(m2·24 h)-1。     

有机硅改性水性聚氨酯增深剂的合成及应用

以异佛尔酮二异氰酸酯(IPDI)和聚丙二醇(PPG,Mn=600)为原料,在催化剂二月桂酸二丁基锡(DBTDL)作用下合成聚氨酯预聚体,经3-氨丙基三乙氧基硅烷(KH-550)改性后,通过1,4-丁二醇(BDO)和三乙醇胺(TEA)扩链,合成了阳离子型有机硅改性水性聚氨酯乳液.讨论了R值[n(—NCO)/n(—OH)]、w(KH-550)以及w(TEA)对乳液性能的影响.利用红外光谱(FT-IR)、核磁共振氢谱(1H-NMR)和Zeta电位表征了增深剂的结构及其性能,并测试了全棉织物和真丝织物经增深剂整理后的性能.结果表明:增深后的黑色全棉织物的增深百分率为19.73%,黑色真丝织物的增深百分率为17.49%,干、湿摩擦牢度提高0.5级以上,整理后织物的耐洗性能比较好.     

无醛有机硅改性聚丙烯酸酯涂料印花黏合剂的制备与应用

选用不含甲醛的交联单体甲基丙烯酸缩水甘油酯(GMA)替代目前常用的N-羟甲基丙烯酰胺(NMA),同时将八甲基环四硅氧烷(D4)及乙烯基三乙氧基硅烷(VTES)偶联剂作为改性单体,对聚丙烯酸酯进行有机硅改性,制备了具有环保性的无醛有机硅改性聚丙烯酸酯涂料印花黏合剂。考察了催化剂、VTES、有机硅单体接枝量和引发剂对单体转化率、凝胶率及黏合剂性能的影响。结果表明,以丙烯酸作催化剂,D4和VTES的质量分数5%(相对丙烯酸单体质量),其中VTES质量分数为1%(相对D4质量),预聚后接枝聚丙烯酸酯,可得到应用性能较佳的有机硅改性聚丙烯酸酯乳液。     

功能性有机硅树脂织物涂层的制备与应用北大核心

将合成的长碳链改性硅树脂RL乳液和纳米杂化有机硅树脂PSO乳液对织物进行涂层整理,测试整理后棉织物的防水性和阻燃性。结果表明:当白炭黑质量分数为2%、n(RL)∶n(PSO)=1∶1.2时,整理织物具有较好的阻燃性和耐水洗性能。     

丙烯酸酯类无氟拒水剂的合成及应用

以甲基丙烯酸十八烷基酯(SMA)、丙烯酸乙酯(EA)、丙烯酸正丁酯(BA)、甲基丙烯酸甲酯(MMA)和丙烯酰胺(AAM)为单体,十六烷基三甲基溴化铵(CTAB)和吐温-20(Tween-20)为复合乳化剂,偶氮二异丁脒盐酸盐(AIBA)为引发剂,采用乳液聚合法制备无氟拒水剂乳液。通过试验得到最佳合成工艺为:复合乳化剂CTAB与Tween-20的质量比为2∶1,乳化剂质量分数为6%(对单体总质量),引发剂质量分数为0.6%(对单体总质量),单体质量分数为30%,反应温度为70℃,反应时间为3 h。该工艺制得的无氟拒水剂乳液性能优异,稳定性好。经该拒水剂整理的涤纶织物对水的接触角约可达135°。     

棉用高效皂洗剂的制备

为了提高棉织物在染色后皂洗过程中的浮色去除能力和抗再沾污能力,并减少含磷废水的排放,采用衣康酸、丙烯酸、N-乙烯基吡咯烷酮作为单体,合成一种高分子皂洗剂。通过测定合成产物的黏度、分散力、螯合力,优化助洗剂的合成工艺为:合成反应温度85℃,单体物质的量之比n(衣康酸)∶n(丙烯酸)∶n(N-乙烯基吡咯烷酮)=1∶5∶0.4,引发剂质量分数为单体总质量的3%,滴加时间2 h,保温时间3 h。经复配,制备出高效皂洗剂。此高效皂洗剂比传统含磷皂洗剂在湿摩擦牢度方面可提升半级,抗再沉积能力值提升4.52。     

氟硅改性丙烯酸酯乳液的合成

以甲基丙烯酸甲酯(MMA)和丙烯酸丁酯(BA)为基础单体,甲基丙烯酸十二氟庚酯G-04和γ-甲基丙烯酰氧基三甲氧基硅烷(KH-570)等为改性单体,在阴/非离子复合乳化剂(2.5%),引发剂(0.7%),交联剂(1%)的作用下,采用乳液聚合方法制备氟硅改性丙烯酸酯乳液。得到的乳液外观较好,对其进行红外光谱表征,加入的有机氟单体和有机硅单体均已接入共聚链段。使用合成的氟硅改性丙烯酸酯乳液对棉织物进行拒水处理,处理后棉织物的水接触角为140°,拒水性能优良。     

改性有机硅防水剂的应用

以八甲基环四硅氧烷(D4)、乙烯基三乙氧基硅烷、长碳链三甲氧基硅烷以及N-β-(氨乙基)-?-氨丙基甲基二甲氧基硅烷为原料合成改性硅油,并乳化为含固量25%的乳液。采用该有机硅防水剂乳液对棉织物进行防水整理,得到优化整理工艺为:乳化剂质量分数3%,乳液p H值5~6,整理剂质量浓度100 g/L,浸渍时间4 min,170℃焙烘3 min。整理织物与水的接触角可达到156.5°,且柔软性增强。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Textural Properties of Cold-set Gels Induced from Heat-denatured Whey Protein Isolates

A 9% whey protein (WP) isolate solution at pH 7.0 was heat-denatured at 80°C for 30 min. Size-exclusion HPLC showed that native WP formed soluble aggregates after heat-treatment. Additions of CaCl2 (10–40 mM), NaCl (50–400 mM) or glucono-delta-lactone (GDL, 0.4–2.0%, w/v) or hydrolysis by a protease from Bacillus licheniformis caused gelation of the denatured solution at 45°C. Textural parameters, hardness, adhesiveness, and cohesiveness of the gels so formed changed markedly with concentration of added salts or pH by added GDL. Maximum gel hardness occurred at 200 mM NaCl or pH 4.7. Increasing CaCl2 concentration continuously increased gel hardness. Generally, GDL-induced gels were harder than salt-induced gels, and much harder than the protease-induced gel.     

Influence des ions sur le pouvoir hydratant de l'ure e: e tude sur peau de porc ex vivo

This study deals with the influence of ions (NaCl and MgSO4) in a W/O emulsion containing 10% urea. Moisturization kinetics are assessed by corneometry on pig skin ex vivo. The formula's influence on urea penetration is measured by infrared spectrometry with an ATR device and the stripping method. Corneometry and spectroscopy were chosen to record simultaneously the hydratation levels and urea localization into superficial cell layers. Urea crystallization after evaporation of emulsions and aqueous solutions is described. Results show that urea does not hydrate nor penetrate when applied to the skin through an aqueous gel. In a W/O emulsion, sodium chloride increases the ability of urea to moisturize without improving penetration. In vitro urea crystallization is disturbed by sodium chloride or magnesium sulphate for solutions and emulsions. This stabilization by ions is correlated with good moisturization values. The stabilization of urea in the solute state provided by ions increases its water epidermal binding capacity without enhancing penetration.     

Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.