- Benzalkonium chloride preparation method
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The invention discloses a benzalkonium chloride preparation method, which comprises: (1) carrying out a salt formation reaction on a fatty alkyl dimethyl tertiary amine and benzyl chloride in an organic solvent at a temperature of 30-70 DEG C to obtain fatty alkyl dimethyl benzyl ammonium chloride, wherein the fatty alkyl is dodecyl, tetradecyl or hexadecyl, and the organic solvent is one or a plurality of materials selected from methanol, ethanol, n-propanol, isopropanol, acetone and acetonitrile; and (2) in an organic solvent, crystallizing the mixture containing two or three fatty alkyl dimethyl benzyl ammonium chlorides prepared in the step (1). According to the present invention, the preparation method has advantages of simple process and high yield, wherein the yield can achieve morethan 90%; the content of the related substance is low, and the purity is high, and can achieve more than 99%; the water content is low; and the product has good appearance and simple post-treatment effect, can meet the requirements of various pharmacopoeia, and is suitable for the industrial production of pharmaceutical-grade benzalkonium chloride.
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Paragraph 0033-0034; 0041-0044
(2019/04/26)
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- Fatty alkyl dimethyl benzyl quaternary ammonium salt synthesis method
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The invention discloses a fatty alkyl dimethyl benzyl quaternary ammonium salt preparation method, which comprises: carrying out a salt formation reaction on fatty alkyl dimethyl tertiary amine and abenzyl halide in an organic solvent at a temperature of 30-70 DEG C, wherein R in the fatty alkyl tertiary amine is C6H13-C22H45, the halogen in the benzyl halide is chlorine, bromine or iodine, and the organic solvent is one or a plurality of materials selected from methanol, ethanol, n-propanol, isopropanol, acetone and acetonitrile. According to the present invention, the yield of the preparation method is high, and can reach more than 90%; the purity is high, and can achieve more than 99%; the water content is low; the product has good appearance and simple post-treatment effect; and the method can reduce the energy consumption, and is suitable for industrial production.
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Paragraph 0043-0046; 0071
(2019/04/26)
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- Benzalkonium chloride monomer synthesis technology
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The invention relates to the technical field of fine chemicals, and more specifically relates to a benzalkonium chloride monomer synthesis technology. The synthesis technology comprises the following steps: (1) according to a formula, weighing fatty alkyl dimethyl tertiary amines, benzyl chloride, and ethyl acetate; (2) adding ethyl acetate into a glass lined reactor, pumping fatty alkyl dimethyl tertiary amines and benzyl chloride into a head tank, starting the stirring device of the reactor, dropwise adding fatty alkyl dimethyl tertiary amines and benzyl chloride into the reactor at a room temperature according to a same ratio; (3) heating the reactor to a temperature of 70 to 100 DEG C, and maintaining the temperature to carry out reactions for 7 to 10 hours; (4) starting circulating cooling water to cool the products to the room temperature until crystals are precipitated completely; (5) taking out the crystals, subjecting the crystals to vacuum suction filtration, during the suction filtration process, washing the crystals by ethyl acetate for 2 to 5 times, and saving the filter cakes; and (6) adding ethyl acetate into the filter cakes, carrying out re-crystallization, and after the crystals are completely precipitated, drying the crystals. The production cost is low and the purity of prepared benzalkonium chloride is high.
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Paragraph 0017; 0022
(2017/09/01)
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- A synthetic method of a benzalkonium chloride mixture
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The invention relates to the technical field of organic synthesis, and particularly relates to a synthetic method of a benzalkonium chloride mixture. The method includes (1) weighing alkyl dimethyl tertiary amine, a metal or nonmetal halide, benzyl chloride and an organic solvent separately according to a ratio; (2) dissolving the alkyl dimethyl tertiary amine and the metal or nonmetal halide into the organic solvent according to a ratio to obtain a mixture system, putting the mixture system in a hydrothermal boiler and raising the temperature of the mixture system to 50-80 DEG C; (3) adding dropwise the benzyl chloride into the mixture system in the step (2) under continuous stirring, with the adding speed being 30-40 drops per min, stirring the mixture system until the dropwise addition is finished, and allowing the obtained mixture system to stand for 3-8 h to obtain benzalkonium chloride single crystals; and (4) subjecting the mixture system in the step (3) to suction filtration, and performing washing operation and recrystallization to obtain the benzalkonium chloride. Compared with traditional processes, the metal or nonmetal halide is adopted as an additive of the method, can promote benzalkonium chloride generation from a reaction of the alkyl dimethyl tertiary amine and the benzyl chloride, and increases the conversion ratio of reactants; and a benzyl chloride dropwise addition manner is adopted by the method, thus reducing benzyl chloride volatilization, allowing the benzyl chloride to be completely reacted as soon as the benzyl chloride is added into a solution, and increasing the conversion ratio of the reactants.
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Paragraph 0017; 0018
(2017/08/30)
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- STABLE COMPOSITIONS OF THIABENDAZOLE AND IODINE-CONTAINING FUNGICIDES
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The present invention relates to stable compositions for the fungicidal equipment of thermoplastic polymers, in particular PVC, comprising thiabendazole, at least one iodine-containing fungicide and at least one epoxide and optionally further fungicidally active compounds, and also to methods for preparing these formulations and to uses thereof for the protection of thermoplastic polymers against attack and destruction by microorganisms. Moreover, the invention relates to mold-resistant PVC materials equipped with the compositions according to the invention.
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- FUNGICIDAL PENFLUFEN MIXTURES
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The invention relates to mixtures comprising penflufen, to the use of these mixtures for protecting industrial materials and to a method for treating industrial materials with the penflufen mixtures.
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- DENTAL ORAL COMPOSITION
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A dental composition for oral use, containing a phosphorylated saccharide (a), a polyphosphoric acid and/or a salt thereof (b), and a cationic bactericidal agent (c), wherein a ratio of a total amount of the phosphorylated saccharide (a) and the polyphosphoric acid and/or a salt thereof (b) contained to an amount of the cationic bactericidal agent (c) contained, i.e. {(a)+(b)}/(c), is from 0.05 to 20 in a weight ratio. The dental composition for oral use of the present invention can be suitably used for an oral cavity cleaning agent, including dentifrice agents such as a paste dentifrice agent, a powder dentifrice agent, and a liquid dentifrice agent, a mouse-wash agent, a troche, a tablet, a cream, an ointment, a bonding agent, a mouth spray, a coating agent to tooth surface or a dental prosthetic, a hypersensitive inhibitor, a therapeutic agent for periodontal diseases, that is applied to a periodontal pocket, wet tissue for oral cavity care, an oral refreshing agent, chewing gum, or a gargling agent, or the like.
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- METHOD FOR PRODUCING ALKYLDIMETHYLBENZYLAMMONIUM CHLORIDES
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The invention is meant for chemical industry and is applicable in production of household sanitizers and detergents. A mixture of commercial tertiary amines or a mixture of straight-run tertiary amines is rectified and fed into the reactor for synthesis of a quaternary ammonium compound by a reaction of said mixture with benzyl chloride under stirring and at an elevated temperature. The mass ratio of the tertiary amines-benzyl chloride mixture is between 1.57 and 1.81. It is preferred that the use is made of benzyl chloride refined by distillation at the atmospheric pressure and a temperature of 177-178° C. The derived quaternary ammonium compound consists essentially of dimethyl dodecyl benzyl ammonium chloride and tetradecyl dimethylbenzyl ammonium chloride, the mass ratio of which is controllable. The product can be obtained in the form of gel. Where water or an organic solvent is added to the reaction mixture, a dissolved product is obtained. The product is free from alkyl radicals with the number of carbon atoms over 14, is low-toxic, and its purity is at least 95 mass %. The proposed invention renders it possible to use inexpensive and procurable raw materials, to lower energy intensity and process time, 1 claim, 1 fig., 3 tabl., 5 emb.
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Page/Page column 4
(2008/06/13)
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- 3-NITROISOXAZOLES AND THEIR USE IN THE PROTECTION OF MATERIALS
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The 3-nitroisoxazoles of the formula (I) in which R1 and R2 are each as defined in the description, some of which are known, are highly suitable for use as biocides for protecting industrial materials.
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- O-aryl dithiazole dioxides
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The invention relates to new O-aryldithiazole dioxides, to two processes for their preparation, and to their use as pesticides in crop protection and in the protection of materials.
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- Interactions between biocide cationic agents and bacterial biofilms
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The resistance of bacterial biofilms to physical and chemical agents is attributed in the literature to various interconnected processes. The limitation of mass transfer alters the growth rate, and physiological changes in the bacteria in the film also appear. The present work describes an approach to determination of the mechanisms involved in the resistance of bacteria to quaternary ammonium compounds (benzalkonium chloride) according to the C-chain lengths of those compounds. For Pseudomonas aeruginosa CIP A 22, the level of resistance of the bacteria in the biofilm relative to that of planktonic bacteria increased with the C-chain length. For cells within the biofilm, the exopolysaccharide induced a characteristic increase in surface hydrophilicity. However, this hydrophilicity was eliminated by simple resuspension and washing. The sensitivity to quaternary ammonium compounds was restored to over 90%. Staphylococcus aureus CIP 53 154 had a very high level of resistance when it was in the biofilm form. A characteristic of bacteria from the biofilm was a reduction in the percent hydrophobicity, but the essential point is that this hydrophobicity was retained after the biofilm bacteria were resuspended and washed. The recovery of sensitivity was thus only partial. These results indicate that the factors involved in biofilm resistance to quaternary ammonium compounds vary according to the bacterial modifications induced by the formation of a biofilm. In the case of P. aeruginosa, we have underlined the involvement of the exopolysaccharide and particularly the three-dimensional structure (water channels). In the case of S. aureus, the role of the three-dimensional structure is limited and drastic physiological changes in the biofilm cells are more highly implicated in resistance.
- Campanac,Pineau,Payard,Baziard-Mouysset,Roques
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p. 1469 - 1474
(2007/10/03)
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- Quaternization reaction of some N,N-dimethylalkylamines with benzyl chloride
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The parameters which influence the quaternization reaction of some N,N-dimethylalkylamines of RN(CH3)2, type (R = octyl, decyl, dodecyl, tetradecyl and hexadecyl) with benzyl chloride were studied. By thermogravimetric analyses, the kinetic parameters, the reaction order, "n", and the activation energy, "Ea", of the thermal decomposition of the quaternary salts prepared in this study, were established.
- Avram, Ecaterina
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- Arylthio-dithiazindioxides and their use as pesticides
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PCT No. PCT/EP97/07242 Sec. 371 Date Jun. 23, 1999 Sec. 102(e) Date Jun. 23, 1999 PCT Filed Dec. 22, 1997 PCT Pub. No. WO98/29400 PCT Pub. Date Jul. 9, 1998The invention relates to novel S-aryl-dithiazine dioxides, to processes for their preparation and to the use in crop protection and in the protection of materials.
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- Termite-controlling agent composition
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Combating termites with a composition comprising (a) at least one compound of the formula STR1 wherein, R denotes a hydrogen atom, acyl, alkyl or optionally substituted heteroarylalkyl, A denotes a hydrogen atom, alkyl or a bivalent group which binds to B, D denotes alkyl, --S--R1, STR2 or bivalent group or atom which binds to A. wherein R1 or R2 each independently denotes a hydrogen atom, acyl, alkyl or optionally substituted heteroarylalkyl. Y denotes =N-- or STR3 wherein T1 denotes a hydrogen atom or optionally substituted alkyl, and X denotes an electron attracting group, and (b) a pyrethoid compound.
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- Fungicidal and bactericidal method
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A fungicidal and bactericidal method of imparting fungicidal and bactericidal properties to an article by coating or impregnating the article with a solution of a quaternary ammonium salt of alginic acid or carboxymethyl cellulose (which is insoluble or sparingly soluble in water) in an organic solvent and thereafter removing the solvent from the article.
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- Production of unsaturated acids, esters and nitriles, and catalyst therefor
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Alkanoic acids, esters of such acids, and alkyl nitriles are reacted with formaldehyde in the presence of a basic catalyst comprising pyrogenic silica to form α,β-unsaturated acids, the esters of such unsaturated acids or α,β-unsaturated nitriles. The pyrogenic silica is especially effective when treated with activating agents which provide basic sites on the pyrogenic silica catalyst support, such as organic bases, inorganic bases of Groups IIA and IIIA metals, and precursors of such bases.
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