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申请号:201911278947.8 公开号:CN110862540A 主分类号:C08G73/10
摘要:【中文】发明公开了一种聚天冬氨酸锌盐的生产方法,具体是由氨水控制体系pH值,水解聚琥珀酰亚胺(PSI)得聚天冬氨酸(PASP),同时在铵盐存在下,溶解氢氧化锌/氧化锌为可溶性Zn(NH3)4(OH)2,与聚天冬氨酸反应生成聚天冬氨酸锌。该方法在水解PSI成PASP的同时,与PASP生成聚天冬氨酸锌,两步反应同时进行,缩短了工时,节约了能耗;此法直接与锌盐反应,避免了聚天冬氨酸钙中间体的使用,缩减了工序和工时,节能降耗,且避免了大量钙盐的产生。该方法无副产,无废物产生,绿色环保,利于实现工业化生产。 【EN】The invention discloses a production method of polyaspartic acid zinc salt, which comprises the steps of controlling the pH value of a system by ammonia water, hydrolyzing Polysuccinimide (PSI) to obtain Polyaspartic Acid (PASP), and dissolving zinc hydroxide/zinc oxide into soluble Zn (NH) in the presence of ammonium salt3)4(OH)2And reacting with polyaspartic acid to generate polyaspartic acid zinc. The method hydrolyzes PSI into PASP, and simultaneously generates polyaspartic acid zinc with PASP, and the two-step reaction is carried out simultaneously, thereby shortening the working hours and saving the energy consumption; the method directly reacts with zinc salt, avoids the use of a calcium polyaspartate intermediate, reduces working procedures and working hours, saves energy, reduces consumption and avoids the generation of a large amount of calcium salt. The method has no byproduct and waste, is green and environment-friendly, and is beneficial to realizing industrial production.
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申请号:201911390824.3 公开号:CN110863069A 主分类号:C14C9/02
摘要:【中文】本发明提供一种以液态顺丁烯二酸酐、不同脂肪链的聚氧乙烯醚、水溶性磺化剂为原料,在矿物油存在的体系中分别经酯化、部分磺化连续合成皮革加脂剂的方法。使用了马来酸作两种脂肪醇聚氧乙烯醚的连接集团,并作为磺化位点,通过磺化反应,利用连续化进料生产方式,稳定产品质量、提高设备利用率,易于实现自动化工业生产;整个过程通过连续转料的方式,实现了物料的自动降温,反应过程易控制、转化率高,反应条件温和,操作安全,易于工业化操作。 【EN】The invention provides a method for continuously synthesizing leather fatting agent by respectively esterifying and partially sulfonating liquid maleic anhydride, polyoxyethylene ethers with different fatty chains and water-soluble sulfonating agents serving as raw materials in a system with mineral oil. Maleic acid is used as a connecting group of two fatty alcohol-polyoxyethylene ethers and a sulfonation site, and a continuous feeding production mode is utilized through sulfonation reaction, so that the product quality is stabilized, the utilization rate of equipment is improved, and the automatic industrial production is easy to realize; the whole process realizes the automatic cooling of the materials by a continuous material transferring mode, the reaction process is easy to control, the conversion rate is high, the reaction condition is mild, the operation is safe, and the industrial operation is easy.
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申请号:201911085249.6 公开号:CN110981908A 主分类号:C07F9/38
摘要:【中文】本发明公开了一种水处理剂氨基三甲叉膦酸的生产方法,具体是将氨水、亚磷酸、盐酸、甲醛按一定比例匀速投入反应釜中,经梯度溢流、保温、冲蒸、稀释等工序,得到高纯度的ATMP水溶液。此法通过连续化投放液体原料,连续化出料的简单操作方式,实现连续化生产,大大缩短了生产周期。此法通过控制反应条件,实现ATMP一次转化率≥98%,无需再分离原料,节约工时和成本。此法所用盐酸为催化剂,经处理后可重复使用,无三废产生,绿色环保。 【EN】The invention discloses a production method of water treatment agent amino trimethylene phosphonic acid, which comprises the steps of uniformly putting ammonia water, phosphorous acid, hydrochloric acid and formaldehyde into a reaction kettle according to a certain proportion, and obtaining high-purity ATMP aqueous solution through the procedures of gradient overflow, heat preservation, flushing evaporation, dilution and the like. The method realizes continuous production and greatly shortens the production period by a simple operation mode of continuously feeding liquid raw materials and continuously discharging materials. The method realizes that the one-time conversion rate of ATMP is more than or equal to 98 percent by controlling reaction conditions, does not need to separate raw materials, and saves working hours and cost. The hydrochloric acid used in the method is used as a catalyst, can be reused after treatment, does not generate three wastes, and is green and environment-friendly.
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申请号:201911390899.1 公开号:CN111040078A 主分类号:C08F226/06
摘要:【中文】本发明公开一种水溶性荧光标记羧酸‑磺酸基共聚物及其合成方法,具体内容包括:(1)将丙烯酸与对甲氧基苯甲酰肼,合成荧光单体,结构如下:;(2)将荧光单体、丙烯酸和2‑丙烯酰胺基‑2‑甲基丙磺酸水溶液,以氧化‑还原引发剂引发聚合,水溶性荧光标记型羧酸‑磺酸基共聚物。本发明利用含碳碳双键的不饱和羧酸与对甲氧基苯甲酰肼经双酰化、脱水一步合成含有不饱和碳碳双键的1,3,4‑恶二唑荧光单体,进一步聚合合成分子量3000~7000的水溶性荧光标记羧酸‑磺酸基共聚物。本发明提供的聚合物激发能量低,浓度荧光线性良好。方法可操作性强,条件温和,溶剂可回收,一步直接反应,易于大规模工业化生产。 【EN】The invention discloses a water-soluble fluorescence labeling carboxylic acid-sulfonic acid group copolymer and a synthetic method thereof, and the specific content comprises the following steps: (1) acrylic acid and p-methoxybenzoyl hydrazine are synthesized into a fluorescent monomer, and the structure is as follows:(ii) a (2) The polymerization is initiated by the fluorescent monomer, acrylic acid and 2-acrylamide-2-methyl propanesulfonic acid aqueous solution by an oxidation-reduction initiator, and the water-soluble fluorescence labeling type carboxylic acid-sulfonic acid group copolymer. The inventionUnsaturated carboxylic acid containing carbon-carbon double bonds and p-methoxybenzoyl hydrazine are subjected to double acylation and dehydration to synthesize a 1,3, 4-oxadiazole fluorescent monomer containing unsaturated carbon-carbon double bonds in one step, and the water-soluble fluorescence-labeled carboxylic acid-sulfonic acid group copolymer with the molecular weight of 3000-7000 is further synthesized through polymerization. The polymer provided by the invention has low excitation energy and good concentration fluorescence linearity. The method has strong operability, mild conditions, recoverable solvent, one-step direct reaction and easy large-scale industrial production.
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申请号:201911395285.2 公开号:CN111039889A 主分类号:C07D271/10
摘要:【中文】本发明公开一种含1,3,4‑恶二唑荧光基团水溶性聚合物及其合成方法,具体内容包括:(1)将丙烯酸与对甲基苯甲酰肼反应得到单体,结构如:;(2)将合成的荧光单体、异丙醇、去离子水与丙烯酸及其它含不饱和双键的水溶性有机单体引发聚合。本发明利用含碳碳双键的不饱和羧酸与对甲基苯甲酰肼经双酰化、脱水一步合成含有1,3,4‑恶二唑荧光基团的荧光单体,并进一步合成粘均分子量在2000~1000范围的标记型荧光聚合物。产品具有优良的水溶性,与荧光单体相比,荧光聚合物的吸收波长发生明显红移,激发能量降低。同时,荧光聚合物的荧光强度与其在水体中的浓度含量呈现良好的线性关系,产品合成工艺安全环保,易于实现工业生产。 【EN】The invention discloses a water-soluble polymer containing 1,3, 4-oxadiazole fluorescent group and a synthesis method thereof, and the specific content comprises the following steps: (1) reacting acrylic acid with p-methylbenzoyl hydrazine to obtain a monomer with the structure as follows:and (2) initiating the polymerization of the synthesized fluorescent monomer, isopropanol, deionized water, acrylic acid and other water-soluble organic monomers containing unsaturated double bonds. The invention further synthesizes a fluorescent monomer containing 1,3, 4-oxadiazole fluorescent group by using unsaturated carboxylic acid containing carbon-carbon double bonds and p-methylbenzoyl hydrazine through double acylation and dehydration, and further synthesizes a labeled fluorescent polymer with the viscosity average molecular weight of 2000-1000. The product has excellent water solubility, and compared with fluorescent monomers, the absorption wavelength of the fluorescent polymer generates obvious red shift, and the excitation energy is reduced. Meanwhile, the fluorescence intensity of the fluorescent polymer and the concentration content of the fluorescent polymer in water body present a good linear relationship, the product synthesis process is safe and environment-friendly, and the industrial production is easy to realize.
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申请号:201911389911.7 公开号:CN110981722A 主分类号:C07C67/08
摘要:【中文】本发明公开了一种含醇丙烯酸甲酯的合成方法及其应用,具体做法如下:将丙烯酸和甲醇按照打入混料釜,然后依次阻聚剂和催化剂,充分搅拌使其混合均匀;然后将混合均匀的物料转入反应塔釜内,保温反应;进行体系外采至精馏塔分离,同时往反应体系中分批次补加甲醇直至反应塔釜内物料回流温度降至约65℃停止循环精馏反应。通过控制反应温度和精馏塔塔顶温度,采用甲醇大量过量的方法将反应形成的甲醇‑丙烯酸甲酯‑水三元混合体系以形成的丙烯酸甲酯‑甲醇共沸体系分离出来。甲醇‑丙烯酸甲酯混合液,直接应用于合成高效水处理剂PBTCA的中间体2‑膦酸二甲酯基‑1,2,4‑丁三酸甲酯,降低生产成本,利于实现反应的连续进行和规模化工业生产。 【EN】The invention discloses a synthetic method of alcohol-containing methyl acrylate and application thereof, and the specific method comprises the following steps: the acrylic acid and the methanol are pumped into a mixing kettle, and then the polymerization inhibitor and the catalyst are sequentially stirred fully to be mixed uniformly; then transferring the uniformly mixed materials into a reaction tower kettle, and carrying out heat preservation reaction; and (3) extracting the mixture outside the system to a rectifying tower for separation, and simultaneously adding methanol into the reaction system in batches until the reflux temperature of the materials in the kettle of the reaction tower is reduced to about 65 ℃ to stop the cyclic rectification reaction. The method is characterized in that a methanol-methyl acrylate-water ternary mixed system formed by reaction is separated out by controlling the reaction temperature and the top temperature of the rectifying tower and adopting a method of large excess of methanol to form a methyl acrylate-methanol azeotropic system. The methanol-methyl acrylate mixed solution is directly applied to synthesizing an intermediate 2-dimethyl phosphonate-1, 2, 4-methyl butanetriacate of the high-efficiency water treatment agent PBTCA, reduces the production cost, and is beneficial to realizing the continuous reaction and the large-scale industrial production.
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申请号:201911391596.1 公开号:CN111097481A 主分类号:B01J29/06
摘要:【中文】本发明公开了一种含钛、氮掺杂石墨烯量子点分子筛的制备方法,具体以钛酸四丁酯为钛源,与N掺杂石墨烯量子点复合,以分子筛为载体,将改性后的钛/氮杂化石墨烯量子点通过化学键稳定附着在分子筛上。通过钛、氮掺杂石墨烯量子点的引入,将二氧化钛的吸收光谱拓展到可见光区,使量子点整体在可见光区的光催化活性明显提高,提高了其对有机物降解的效率,降低了降解时间;钛氮原子促进电荷转移,抑制光生电子‑空穴的复合,提高了量子点的光催化效率;分子筛的引入,可吸附水体中重金属离子和有机物质,有机物直接被附着的钛/氮杂化石墨烯量子降解,保证了体系的降解稳定性和效率,也便于光催化剂的回收,节约成本。 【EN】The invention discloses a preparation method of a titanium and nitrogen-containing doped graphene quantum dot molecular sieve, which specifically comprises the steps of taking tetrabutyl titanate as a titanium source, compounding with N-doped graphene quantum dots, taking the molecular sieve as a carrier, and stably attaching modified titanium/nitrogen-doped graphene quantum dots to the molecular sieve through chemical bonds. By introducing the titanium and nitrogen doped graphene quantum dots, the absorption spectrum of titanium dioxide is expanded to a visible light region, so that the photocatalytic activity of the quantum dots in the visible light region is obviously improved, the organic matter degradation efficiency is improved, and the degradation time is reduced; the titanium nitrogen atoms promote charge transfer, inhibit the recombination of photoproduction electrons and holes and improve the photocatalytic efficiency of the quantum dots; the introduction of the molecular sieve can adsorb heavy metal ions and organic substances in a water body, and organic substances are directly degraded by the attached titanium/nitrogen hybridized graphene quantum, so that the degradation stability and efficiency of a system are ensured, the recovery of the photocatalyst is facilitated, and the cost is saved.
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申请号:201911308979.8 公开号:CN111087422A 主分类号:C07F9/38
摘要:【中文】本发明公开了一种减水剂单体(2‑膦酸‑亚丙基)丙二酸的制备方法,具体使用异丙烯膦酸和丙二酸通过迈克尔加成,氯化,脱氯化氢等反应步骤,合成(2‑膦酸‑亚丙基)丙二酸,实现了单元内膦酸基和羧基的共存,(2‑膦酸‑亚丙基)丙二酸继续和烯基聚氧乙烯醚大单体聚合制备的聚羧酸系减水剂,不但具有高分散性,高坍落保持性,且缓凝效果突出,适应多种使用低活性填料制备的混凝土,同时还有效降低了减水剂的单位用量。 【EN】The invention discloses a preparation method of (2-phosphonic acid-propylene) malonic acid as a water reducer monomer, which specifically comprises the steps of carrying out Michael addition, chlorination, dehydrochlorination and other reaction steps on isopropenylphosphonic acid and malonic acid to synthesize the (2-phosphonic acid-propylene) malonic acid, so that coexistence of phosphonic acid groups and carboxyl groups in units is realized, and the (2-phosphonic acid-propylene) malonic acid is continuously polymerized with an alkenyl polyoxyethylene ether macromonomer to prepare a polycarboxylic water reducer.
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申请号:201911389909.X 公开号:CN111072829A 主分类号:C08F122/06
摘要:【中文】本发明提供了一种聚马来酸的合成方法,具体是以水相为介质,将过氧化氢滴加到顺丁烯二酸酐水溶液中聚合反应,通过电解作用,提高低浓度体系中过氧化氢的利用率和自由基引发速率效率,减少引发剂过氧化氢的用量,缩短反应时间,降低成本。实现了使用过氧化氢做引发剂的水相聚合,反应无需使用其他金属催化剂或助剂,避免了金属类催化剂的环境污染问题。 【EN】The invention provides a method for synthesizing polymaleic acid, which particularly takes a water phase as a medium, hydrogen peroxide is dripped into a maleic anhydride aqueous solution for polymerization, the utilization rate of the hydrogen peroxide in a low-concentration system and the free radical initiation rate efficiency are improved through electrolysis, the dosage of the initiator hydrogen peroxide is reduced, the reaction time is shortened, and the cost is reduced. The water-phase polymerization using the hydrogen peroxide as the initiator is realized, other metal catalysts or auxiliaries are not needed in the reaction, and the problem of environmental pollution caused by metal catalysts is avoided.
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申请号:201911391589.1 公开号:CN111072842A 主分类号:C08F220/06
摘要:【中文】本发明公开一种含吡啶基1,3,4‑恶二唑水溶性荧光聚合物及其合成方法,具体包括:(1)将丙烯酸与4‑甲酰肼吡啶在干燥的三氯氧磷环境体系中,负压加热回流反应5~6小时,得荧光单体;(2)将合成的荧光单体、丙烯酸和顺丁烯二酸酐水溶液引发聚合,合成粘均分子量为5000~10000的水溶性荧光标记丙烯酸‑马来酸共聚物水溶液。本发明利用含碳碳双键的不饱和羧酸与含吡啶基的1,3,4‑恶二唑的甲酰肼合成含有不饱和碳碳双键的荧光单体,进一步聚合成水溶性荧光标记共聚物;该方法工艺简单易操作、激发能量低,浓度荧光线性好,反应条件温和,合成工艺安全环保、易于实现规模化工业生产。 【EN】The invention discloses a water-soluble fluorescent polymer containing pyridyl 1,3, 4-oxadiazole and a synthesis method thereof, and the water-soluble fluorescent polymer specifically comprises the following steps: (1) heating acrylic acid and 4-formylhydrazinopyridine in a dry phosphorus oxychloride environment system under negative pressure for reflux reaction for 5-6 hours to obtain a fluorescent monomer; (2) and (3) initiating polymerization of the synthesized fluorescent monomer, acrylic acid and maleic anhydride aqueous solution to synthesize a water-soluble fluorescence-labeled acrylic acid-maleic acid copolymer aqueous solution with the viscosity-average molecular weight of 5000-10000. The invention utilizes unsaturated carboxylic acid containing carbon-carbon double bond and formylhydrazine of 1,3, 4-oxadiazole containing pyridyl to synthesize fluorescent monomer containing unsaturated carbon-carbon double bond, and further polymerize into water-soluble fluorescent labeled copolymer; the method has the advantages of simple and easy operation, low excitation energy, good concentration fluorescence linearity, mild reaction conditions, safe and environment-friendly synthesis process and easy realization of large-scale industrial production.
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