专利配方

用过期发射药合成高吸水性树脂的方法用过期发射药合成高吸水性树脂的方法是一种利用过期发射药及其制品合成高吸水性树脂的方法,其合成的方法为:a.将丙烯酸钠用水稀释,b.将废胶棉用丙酮溶胀成稀糊状,c.将溶胀成稀糊状的过期发射药边搅拌边加入到用水稀释后的丙烯酸纳中,d.在以上的材料中加入过氧化氢、亚硫酸氢钠、环氧氯丙烷的乙醇溶液,e.在氮气保护下升温至35℃～45℃,恒温20～40分钟,f.再升温至60℃～90℃静聚合1.5～3小时,烘干,粉碎得最终产品;在合成的过程中,各种原材料按重量百分比计,其配比为:丙烯酸钠49～90%、过期发射药9～48%、过氧化氢0.1～1%、亚硫酸氢钠0.1～1%、环氧氯丙烷0.01～1%,该方法使废物弃的过期发射药得到妥善的回收和再利用,变废为宝。(CN1388142)     

不对称相转移催化合成光活性α-氨基酸

利用不对称相转移催化反应 ,由芳醛或环酮、氯仿和氨合成了 8个光活性α-氨基酸、收率为 2 5 .1 %～ 72 .4% ,比旋光度在± 2 .7～± 5 .5     

羟丙基田菁胶一步水媒法合成工艺研究

自主创新研制出一步水媒法合成羟丙基田菁胶工艺,合成反应不是针对田菁胶粉而是针对胚乳片进行,直接粉碎加工得到羟丙基田菁胶.考察了合成过程中氢氧化钠、环氧丙烷、反应温度、反应时间等因素对产品粘度和水不溶物的影响,获得理想的工艺条件:氢氧化钠、环氧丙烷与胚乳片的质量比分别为0.30:1和0.50:1,反应温度为75～80℃,反应时间为120～130min.合成的羟丙基田菁胶,水不溶物为8%～10%,粘度为1500～2000mPa.s,在粘度与田菁胶原粉基本一致的情况下,水不溶物由30%～35%显著降低到8%～10%.采用该工艺生产的羟丙基田菁胶已经成功地应用于造纸行业.     

Ln/TiO2催化剂的制备研究

目前中国广泛采用以三氧化二铝为载体、以金属盐作活性组分制备合成甲基异丙基酮的催化剂.合成甲基异丙基酮的关键是催化剂的制备技术.为了改善催化剂的选择性,提高合成产物的收率,以异丁酸和乙酸为原料、以In/TiO2为催化剂合成甲基异丙基酮.研究了催化剂活性组分、催化合成反应温度、原料异丁酸和乙酸的配比、催化剂的再生等因素对催化合成反应的影响.确定了合成甲基异丙基酮的最佳条件:稀土活性组分的质量分数15.0%,合成温度430～450℃,异丁酸与乙酸的物质的量比1.0:1.5,反应空速0.6～0.7h-1.在此条件下转化率>90%,催化剂选择性>80%.     

β-葡萄糖五乙酸酯的合成

以吡啶为催化剂,利用葡萄糖和乙酸酐的酯化反应合成了β-葡萄糖五乙酸酯,研究了合成的最佳反应条件和粗产品的结晶条件.结果表明最佳条件为:乙酸酐与葡萄糖的物质的量比为1:6,催化剂的用量为葡萄糖质量的2%,反应时间为3 h.结晶溶剂为乙醇,结晶温度为30℃,乙醇与粗产品的体积比为2:1;葡萄糖与醋酐的酯化收率这9%,β-葡萄糖五乙酸酯的总收率为75.2%.产品的比旋光度 4～ 60°熔点130-134℃.质量分数≥98%(GC).该方法选择性好、产物收率高.     

在硫酸钠熔盐中合成莫来石的热力学研究

以硫酸铝和二氧化硅为原料,以硫酸钠为介质合成莫来石粉体.利用差示扫描量热法研究了合成过程中的热量变化.由理论数据与实验数据分别经过计算得到的反应热变化基本一致,从而确定了合成反应的温度范围应在950～1 000℃之间.利用X射线衍射仪和场致发射扫描电子显微镜等手段对合成粉体的相组成、结构和形貌进行了研究.结果表明:在1 000℃保温3 h合成的莫来石粉体基本无其他相存在,其粉体呈针状晶须,直径约50～100 nm,长度约3～8 um.该方法工艺简单,合成温度较其它方法低200～400℃.     

硅藻土精制副产硫酸铝母液合成聚合铝的研究

研究了利用硅藻土精制副产的硫酸铝母液生产聚合铝的工艺。合成PAS的条件为 :反应温度 40～ 5 0℃ ,熟化温度 35～ 5 0℃ ,熟化时间 3～ 5h ,稳定剂PE - 2用量为 4%～ 5 %。合成PAC -S的条件为 :反应温度 5 0～ 6 0℃ ,熟化温度 35～ 5 0℃ ,熟化时间 3～ 5h ,CaCl2 /CaO比为 2 .5∶1～ 3∶1,添加剂A -Ⅰ用量为 6 %～ 8%。合成过程简单 ,成本低。     

双(3-烷氧基-2-羟基)丙基双季铵盐阳离子表面活性剂的合成与表征

以长链烷基醇、四甲基乙二胺和环氧氯丙烷为原料,经一步反应合成了双季铵盐阳离子表面活性剂(BQAS)。研究了反应时间、反应温度对BQAS产率的影响,确定了合成目标产物的最佳反应时间为24～32h、反应温度为70～80℃,其产率达70.2%～83.3%。目标产物结构通过IR和1HNMR确证。利用吊环法测定目标产物的水溶液在20℃的表面活性,临界胶束浓度(CMC)为7.6×10-6～9.5×10-4mol.L-1,表面张力(γCMC)为34.2～40.6mN.m-1。     

水溶性聚氨酯堵料制备与性能表征

以甲苯二异氰酸酯(简称TDI)与共混聚醚为原料,合成了水溶性聚氨酯的预聚体,并利用FTIR对其结构进行了简单表征.通过分析反应过程中的反应时间及温度对预聚体合成中NCO%的影响,选择了预聚体较佳的合成条件;探讨了不同聚醚配比和溶剂含量对堵料性能的影响.实验结果表明:当预聚体中加入20%溶剂时,共混聚醚化学灌浆具有良好的物理性能,其黏度为141 mPa·s,膨胀率为400%～530%,抗压强度为1.49 MPa,伸长率为150%～218%,灌材凝胶时间可调,对pH值变化的水质有很好的适应能力,而且有很大的包水量.通过凝胶体的形态分析表明,材料发泡均匀且密度大,有非常好的防渗和防水堵漏效果.     

二甲基二硫的合成新工艺

多硫化钠与硫酸二甲酯(DMS)反应合成二甲基二硫(DMDS),考察了原料配比、反应温度、反应时间对反应产物收率的影响,以n(硫磺)∶n(硫化钠)∶n(水)=1∶1.6∶32配成溶液,与硫酸二甲酯在60～75 ℃条件下反应2～2.5 h.总收率为91.6%.二甲硫醚收率仅为1.46%,该三废可以回收利用,易于实现清洁生产.     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

Novel polyurethane coating technology through glycidyl carbamate chemistry

Glycidyl carbamate chemistry combines the excellent properties of polyurethanes with the crosslinking chemistry of epoxy resins. Glycidyl carbamate functional oligomers were synthesized by the reaction of polyfunctional isocyanate oligomers and glycidol. The oligomers were formulated into coatings with several amine functional crosslinkers at varying stoichiometric ratios and cured at different temperatures. Properties such as solvent resistance, hardness, and impact resistance were dependent on the composition and cure conditions. Most coatings had an excellent combination of properties. Studies were carried out to determine the kinetics of the curing reaction of the glycidyl carbamate functional oligomers with multifunctional and model amines. Detailed kinetic analysis of the curing reactions was also undertaken. The results indicated that the glycidyl carbamate functional group is more reactive than a glycidyl ether group. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, on October 27–29, 2004, in Chicago, IL.     

Highly moisture-proof polysilsesquioxane coating prepared via facile sol-gel process

A highly moisture-proof polysilsesquioxane coating was obtained from a new bis-silylated precursor, which was synthesized from 3-aminopropyltriethoxysilane (APTES) and m-xylylene diisocyanate (m-XDI) in tetrahydrofuran (THF) and verified by ¹H MAS NMR. For direct comparison purposes, an SiO₂ coating was also prepared by the Stöber method using tetraethoxysilane (TEOS) as the reactant. Interestingly, the coating obtained from the polysilsesquioxane sol exhibited a much higher moisture resistance capability than its counterpart, which was attributed to its more compact feature between nanoparticles as characterized by N₂ absorption experiment and transmission electron microscopy (TEM). Furthermore, its high transparency of about 92% showed potential for application in the protection of optical crystals.