The method of obtaining fire-resistant fluids

 

(57) Abstract:

The invention relates to the field of chemistry of organophosphorus compounds and can be used to produce fire-resistant hydraulic and lubricating fluids used in power, metallurgical, coal, machine building and other industries, for example in control systems and lubrication of steam turbines, hydraulic coal mining machines, hydraulic machines, injection molding, etc., When a method of producing fire-resistant fluid, comprising the esterification of phosphorus-containing compounds with a mixture of synthetic 3,5-and/ or 3,4-Xylenol and phenol in the presence of a catalyst, and this mixture are in a ratio of components: 3,5-and/or 3,4-Xylenol 80-85 wt.%, phenol 15-20 wt.%. The expected technical result of the invention is to allow the complete exclusion of the composition of the raw material fraction coke xylenols for maintaining the final product physico-chemical, operational and Toxicological properties that meet all the requirements for fire-resistant hydraulic and lubricating materials. table 2.

The invention relates to the field of chemistry fosfororganicheskimi in energy, steel, coal, machine building and other industries, for example, control systems and lubrication of steam turbines, hydraulic coal mining machines, hydraulic machines, injection molding, etc.

To fire-resistant fluids used in these systems is subject to strict requirements on a number of characteristics, including resistance to water (hydrolytic stability), oxidative stability, temperature samosatene, air release properties, are determined by the deaeration (release fluid from the air), viscosity, pour point, which is especially important in the operation of fire-resistant fluids in winter conditions.

A method of obtaining fire-resistant fluids based on trixylenyl phosphate [1] According to this method, a compound of phosphorus (for example, cloroxed phosphorus, phosphoric acid, etc.,) etherification in the presence of a catalyst xylenols fraction of the product refining of fossil fuels with temperature boiling range within 212-222oC (fraction of coke xylenols containing 65-75 3-5-Xylenol, followed by separation of the resulting product fractions con the numerical requirements including toxicity, the level of which does not exceed the level of toxicity of mineral turbine oils.

The disadvantages of this method include the fact that one of the most important operational characteristics of the obtained product, the viscosity can be adjusted within wide limits depending on customer requirements, as most of it is determined by the properties of the selected coke feedstock. In addition, due to the high scarcity of coking raw material that is associated with a decrease in the extraction and processing of fossil fuels required quality specified by the known method cannot ensure the production of fire-resistant fluids in amounts that meet the needs of industry.

A method of obtaining fire-resistant fluid, comprising the esterification of phosphorus-containing compounds with a mixture of synthetic 3,5-Xylenol, phenol and faction coke xylenols (the same as in method [1]) in the presence of a catalyst [2] This known method, by variation of the ratio of components of the raw material makes it possible to adjust the viscosity of the final product (which is a mixture of triarylphosphines different composition) at high values of the other service is elenelov is 19-22 wt. of the total raw materials). With the exception of the composition of the raw material specified fraction of this known method does not.

Attempt complete elimination of the organic components of the raw material by a known method [2] faction coke xylenols due to a corresponding increase in the share of synthetic 3,5-and/or 3,4-Xylenol leads to a significant increase in the content in the composition of the resulting mixture of triarylphosphines di-3,5 - and/or 3,4-seleniferous, which causes crystallization of the final product.

The expected technical result of the invention is to allow the complete exclusion of the composition of the raw material fraction coke xylenols for maintaining the final product physico-chemical, operational and Toxicological properties that meet all the requirements for fire-resistant hydraulic and lubricating materials.

According to the invention this is achieved in that in a method of producing fire-resistant fluid, comprising the esterification of phosphorus-containing compounds with a mixture of synthetic 3,5 - and/or 3,4-Xylenol and phenol in the presence of a catalyst, and this mixture are in the following ratio component is ω demonstrates compliance of the claimed invention, the criterion of "novelty".

A causal relationship between the features and the technical result of the claimed invention lies in the fact that, as shown by experimental studies, this ratio of components of the raw material content in the final product di-3,5 - and/or 3,4-seleniferous does not exceed 30% that does not lead to crystallization of the final product, all physico-chemical and operational properties of the obtained flame-retardant liquids required to meet it requirements.

When searching for additional analogues revealed no known population of the distinctive features of the first claim of the claimed invention as an independent technical solutions that may be evidence of compliance with a criterion of "inventive step".

The possibility of industrial use in thermal power plants and other industrial facilities demonstrates compliance invention, the criterion of "industrial applicability".

The proposed method of producing fire-resistant fluid is as follows. Cloroxed phosphorus is placed in a reaction vessel and perform the esterification in the presence of a catalyst mixture consisting which can be used any of known esterification catalysts (duration 12-15 h), the resulting reaction mass is subjected to distillerie at a pressure of 1.3-1.5 kPa and the temperature range 250-270oC select the target fraction, washed her with an aqueous solution of alkali, then with water until neutral and dried at a temperature of 105-110oC and a pressure of 1.3 to 2.0 kPa.

Example 1. Cloroxed phosphorus is placed in a reaction vessel and etherification mixture consisting of the following components, wt. synthetic 3,5-Xylenol 80; phenol 20, at 140oC in the presence of a catalyst of titanium tetrachloride within 12 hours the reaction mass distil at a pressure of 1.3 to 1.6 kPa, taking fraction in the temperature range 250-270oC. Selected fraction is washed first 3 wt. NaOH solution, and then water washed until neutral, then dried at 105oc and a pressure of 1.3 to 1.6 kPa. Control of the degree of purification are carried out by the acid number and the content of free phenols. The results of the tests of the final product are given in table. 1.

Example 2. The inventive method is carried out analogously to example 1, but for the esterification of chloroxine phosphorus, a mixture consisting of the following components, wt. synthetic 3,4-Xylenol 85; phenol 15.

The results of the final test is for the esterification of chloroxine phosphorus use a mixture, consisting of the following components, wt. synthetic 3,5-Xylenol 55; synthetic 3,4-Xylenol 28; phenol 17.

The results of the tests of the final product are given in table. 1.

Example 4. The inventive method is carried out analogously to example 1, but for the esterification of chloroxine phosphorus, a mixture consisting of the following components, wt. synthetic 3,5-Xylenol 27; synthetic 3,4-Xylenol 57; phenol 16.

In table.1 shows the results of tests of fire resistance fluids, obtained by the proposed method in table. 2 comparison of characteristics and properties of fire-resistant fluids, obtained by the proposed and conventional methods.

Obtained in accordance with the invention of fire-resistant fluids, as can be seen from the table. 1 and 2, despite the absence in the feedstock fraction of coke xylenols have characteristics that meet the requirements of industrial used fire-resistant fluids of similar purpose.

The method of obtaining fire-resistant fluid by the esterification of phosphorus oxychloride are heated in the presence of a catalyst mixture containing a synthetic Xylenol and phenol, characterized in that the process
Phenol 15 20$

 

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The working fluid // 2009185
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FIELD: organic synthesis.

SUBSTANCE: invention relates to synthesis of organophosphorous compounds bearing P-C bond, in particular to preparation of novel 2-dichloromethylenecyclohexylphosphonic acid dichloride (formula I: comprising reaction of 2-alcoxy-7,7-dichlorobicyclo[4.1.0]heptane with phosphorus trichloride in presence of aluminum trichloride used at molar ratio 1:1:1 or 1:2:1, followed by treatment of resulting complex with water in dichloromethane.

EFFECT: increased choice of organophosphorous compounds for use as intermediates in organophosphorous synthesis.

4 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes a method for preparing 7,7-dichlorobicyclo[4,1,0]heptyl-2-phosphonic acid dichloroanhydride of the formula (1):

. Method for preparing 7,7-dichlorobicyclo[4,1,0]heptyl-2-phosphonic acid dichloroanhydride of the formula (1) involves interaction of dichlorobicyclo[4,1,0]heptane with phosphorus trichloride taken in the mole ratio = 1:2 in the presence of oxygen. Synthesized compound represents a valuable semi-finished product used in synthesis of organophosphorus substances.

EFFECT: improved preparing method, expanding assortment of organophosphorus compounds.

2 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for synthesis of 2,4-dichloro-2-dichlorophosphorylbutanoic acid chloroanhydride of the formula: . Method involves interaction of phosphorus pentachloride with γ-butyrolactone in inert organic solvent medium followed by formation of intermediate adduct of phosphorus pentachloride and γ-butyrolactone that then is treated with sulfur-containing compound up to preparing the end product. As a sulfur-containing compound the method involves using sulfuryl chloride, and treatment is carried out at temperature above 25°C. Method provides simplifying process and enhanced yield of the end product.

EFFECT: improved preparing method.

1 ex

FIELD: organic chemistry, biochemistry, medicine.

SUBSTANCE: invention relates to phosphonic acid compounds used as inhibitors of serine proteinase of the general formula (I): wherein R1 is chosen from group comprising piperidinyl, pyrrolidinyl and 1,3,8-triazaspiro[4,5]dec-8-yl (wherein heterocyclic ring as added to nitrogen atom in ring) and -N(R7R80 wherein this heterocyclic ring is substituted optionally with one or two substitutes chosen independently from group comprising the following compounds: (a) C1-C8)-alkyl substituted optionally at terminal carbon atom with a substitute chosen from group comprising aryl, heteroaryl; c) phenyl and naphthalenyl; i) benzothiazolyl; R7 is chosen from group comprising hydrogen atom and (C1-C8)-alkyl; R8 is chosen from group comprising: (aa) (C1-C8)-alkyl; (ab) cycloalkyl; (ac) cycloalkenyl, and (ad) heterocyclyl (wherein R8 is added to carbon atom in ring) wherein (ab) cycloalkyl; (ac) cycloalkenyl, and (ad) heterocyclyl (wherein heterocyclyl (ad) comprises at least one cyclic nitrogen atom) substitutes and cycloalkyl moiety (aa) of a substitute is substituted optionally with substitutes chosen independently from group comprising: (ba) (C1-C8)-alkyl substituted at terminal carbon atom with a substitute chosen from group comprising amino-group (with two substitutes chosen independently from group comprising hydrogen atom and (C1-C8)-alkyl); (bb) (C1-C8)-alkoxy-group substituted at terminal carbon atom with a substitute chosen from group comprising carboxyl; (bc) carbonyl substituted with a substitute chosen from group comprising (C1-C8)-alkyl, aryl, aryl-(C2-C8)-alkenyl; (bd) aryl; (be) heteroaryl; (bf) amino-group substituted with two substitutes chosen independently from group comprising hydrogen atom and (C1-C8)-alkyl; (bh) halogen atom; (bi) hydroxy-group; (bk) heterocyclyl wherein (bd) is aryl substitute, and heteroaryl moiety (bc) comprise a substitute (halogen atom)1-3; R4 is chosen from group comprising aryl and heteroaryl wherein heteroaryl comprises halogen atom as a substitute; R2 and R3 are bound with benzene ring and represent hydrogen atom, and R2 and R3 form in common optionally at least one ring condensed with benzene ring forming polycyclic system wherein this polycyclic system is chosen from group comprising (C9-C14)-benzocondensed cycloalkenyl, (C9-C14)-benzocondensed phenyl; R5 is chosen from group comprising hydrogen atom and (C1-C8)-alkyl; R6 is chosen from group comprising (C1-C8)-alkyl and hydroxy-group; Y is absent, and X represents a single substitute that is added by a double bond and represents oxygen atom (O), and Z is chosen from group comprising a bond, hydrogen atom, and its salts. Also, invention relates to a method for synthesis of these compounds, to their composition inhibiting serine proteinase and to a method for its preparing. Proposed invention describes a method for treatment of inflammatory or serine proteinase-mediated disorder.

EFFECT: valuable biochemical and medicinal properties of compounds.

64 cl, 5 tbl, 38 ex

FIELD: chemistry.

SUBSTANCE: method includes interaction of allylmethallyl ester with phosphorus pentachloride at temperature 0-10°C and their molar ratio 1:2 with further procession of resulting adduct with acetone.

EFFECT: obtaining novel phosphorus-containing compound.

1 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: present invention pertains to the method of producing dichloroanhydride of styryl phosphonic acid and can be used in chemical industry in the production of organic phosphorus compound preproducts. The method involves reacting styrene with phosphorous pentachloride in an inert solvent and disintegration of the obtained styrene adduct using a carbonyl compound. The method is distinguished by that, the carbonyl compound used is urea or its derivatives, and disintegration of the adduct takes place at room temperature.

EFFECT: design of a new efficient method of producing dichloroanhydride of styryl phophonic acid.

1 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method for synthesis of dichloranhydride of 2-(2,3-dichloropropoxy)ethenyl phosphonic acid of formula (1), which can be used in organic synthesis: ClCH2CHClCH2OCH=CHP(O)Cl2, 1. The proposed method involves reaction of vinyl glycidyl ether with phosphorus pentachloride in molar ratio 1:2 in a medium of an inert organic solvent at temperature 0-20°C and subsequent treatment of the formed adduct with acetone.

EFFECT: design of a method for synthesis of an organic synthesis intermediate product.

1 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing N-trimethylsilylamido-chloroanhydride of methyl-phosphonic acid of formula CH3P(O)(Cl)NHSi(CH3)3 and can be used in organic synthesis. The disclosed method of producing N-trimethylsilylamido-chloroanhydride of methyl-phosphonic acid involves reacting dichloroanhydride of methyl-phosphonic acid with hexamethyldisilazane at 60-70°C for 4-6 hours without a solvent.

EFFECT: obtaining a new reagent for organic synthesis.

1 cl, 2 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing physiologically active 6-(N-alkylfluorophosphonyloxy)-5,5-dialkyl-6-aza-7-substituted bicyclo[2.2.1]-heptene-2 of general formula: , where X- CH2, O; R1=CH3, i-C3H7, i-C4H9; R2=H, CH3 C2H5, i-C3H7, i-C4H9, . The disclosed method lies in obtaining the target substance by reacting difluoroanhydride of methyl-phosphonic acid with 6-(N-trimethylsilyloxy)-5,5-dialkyl-5-aza-7-substituted bicyclo[2.2.1]-heptene-2 of general formula , where X, R1 and R2 are given above, at 20-25°C for 0.5-2 hours.

EFFECT: design of a method of obtaining novel physiologically active compounds.

1 cl, 1 ex, 4 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to 2-(N-methylalkoxyphosphonyl)-2-aza-3-thiooxybicyclo[2.2.1]heptene-5 of general formula: , where R=i-C3H7, C4H9, i-C4H9, which have zoocide activity, and a method of producing said compounds. The disclosed method lies in treating corresponding methyl-phosphonic acid thionylamide esters with cyclopentadiene in a benzene solution while boiling for 4-5 hours.

EFFECT: design of a method of obtaining novel biologically active compounds.

2 cl, 2 ex, 2 tbl

FIELD: synthesis of lubricant oil additives.

SUBSTANCE: method for production of O-(n-butyl)-O-3,4,5-trithiatricyclo-dez-8-yl-methyl)-dithiophosphoric acid 1-(N,N-dimethylaminomethyl)-1,2,4-triazole salt of general formula

is disclosed. 1-(N,N-dimethylaminomethyl)-1,2,4-triazole is brought into reaction with equimolar amount of O-(n-butyl)-O-3,4,5-trithiatricyclo-dez-8-yl-methyl)-dithiophosphoric acid in toluene medium at 80-100°C for 2-4 h.

EFFECT: ash-free antiscoring lubricant oil additive operating under high pressure.

2 tbl, 1 ex

FIELD: synthesis of lubricant oil additives.

SUBSTANCE: method for production of O-(2-ethyl-n-hexil)-O-3,4,5-trithiatricyclo[5.2.1.02,6]-dez-8-yl-methyl)-dithiophosphoric acid 1-(N,N-dimethylaminomethyl)-1,2,4-triazole salt of general formula

is disclosed. 1-(N,N-dimethylaminomethyl)-1,2,4-triazole is brought into reaction with equimolar amount of O-(2-ethyl-n-hexyl)-O-3,4,5-trithiatricyclo[5.2.1.02,6]-dez-8-yl-methyl)-dithiophosphoric acid in toluene medium at 80-100°C for 2-4 h.

EFFECT: ash-free antiscoring lubricant oil additive operating under high pressure.

2 tbl, 1 ex

FIELD: synthesis of lubricant oil additives.

SUBSTANCE: method for production of O-(2-ethyl-n-hexil)-O-3,4,5-trithiatricyclo-dez-8-yl-methyl)-dithiophosphoric acid 1-(N,N-dimethylaminomethyl)-benzotriazole salt of general formula 2 is disclosed. 1-(N,N-dimethylaminomethyl)-benzotriazole is brought into reaction with equimolar amount of O-(2-ethyl-n-hexyl)-O-3,4,5-trithiatricyclo-dez-8-yl-methyl)-dithiophosphoric acid in toluene medium at 80-100°C for 2-4 h.

EFFECT: ash-free antiscoring lubricant oil additive operating under high pressure.

2 tbl, 1 ex

FIELD: synthesis of lubricant oiliness addends.

SUBSTANCE: claimed method includes reaction of equimolar amounts of 1-(N,N-dimethylaminomethyl)-benzotriazol and O-(n-butyl)-O-(3,4,5-trithiatricyclodez-8-yl-methyl))-dithiophosphoric acid at 80-100°C in toluene medium for 2-4 h to produce target product of general formula:

.

EFFECT: ash-free addend for lubricant oils processing under high pressure, in particular lubricant oiliness addend of improved antiscoring properties.

2 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: composition contains the following in wt %: a) one or more phosphoric esters 10-85; b) one or more carboxylic esters 5-60; c) one or more C6-C22 fatty acids, possibly ethoxylated with 1-20 moles of ethylene oxide 0.1-30; and/or d) one or more C6-C22 fatty acids, possibly ethoxoylated with 1-20 moles of ethylene 0.1-30; e) water - up to 100. The lubricant composition is used in form of an aqueous composition diluted 2-10000 times on volume. Lubricant compositions can be used in conveyor systems for glass and/or plastic bottles, such as polyethylene terephthalate (PET) or polycarbonate (PC); tin cans, glass containers, casks, cardboard containers and similar articles.

EFFECT: low coefficient of friction for glass, as well as polyethylene terephthalate bottles.

19 cl, 11 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a lubricant composition of noncombustible working (hydraulic) fluid which contains a base which is based on a mixture of phosphoric esters, containing 67.0-73.0 wt % tributyl phosphate, 19.0-25.0 wt % dibutyl phenyl phosphate and 7.0-9.0 wt % triisobutyl phosphate, and a synergetic mixture of additives. The composition of additives includes a thickener additive - polybutyl methacrylate with molecular weight of 5000-6500, epoxy resin, an anticorrosion additive - Chromoxan B, a stabilising additive - Irganox 1010 FF, an oxidation inhibitor - Irganox L 57, a corrosion inhibitor - 1,2,3-benzotriazole, a metal passivating agent - Amino O and a dye, in defined ratios.

EFFECT: obtaining a lubricant composition of noncombustible working fluid with high explosion and fire safety for aviation equipment, which provides stable operation of hydraulic systems.

1 cl, 4 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to an unleaded lubricant for use in hot pressing of metals, which contains 15-40 wt % one or more oils, 3-20 wt % graphite, having particle size distribution for 90% of the particles with size smaller than 15 mcm, and 30-80 wt % one or more phosphoric esters. The present invention relates to a method for hot pressing aluminium or aluminium alloy.

EFFECT: providing excellent lubricating properties and reduced smoke formation and inflammability at temperature of 300°C or higher.

11 cl, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to an explosion- and fire-safe working fluid which contains a mixture of phosphoric esters, which includes tributyl phosphate, dibutyl phenyl phosphate and triisobutyl phosphate, and additives - polybutyl methacrylate, epoxy compound 3,4-epoxycyclohexymethyl-3,4-epoxycyclohexyl carboxylate, anti-erosion additive, oxidation inhibitors, including 2,6-di-tert-butyl-4-methyl-phenol, 1,2,3-benzotriazole and a dye, wherein the mixture of phosphoric esters further includes trixylenyl phosphate; the anti-erosion additive is 4-trifluoromethylperfluoro-3,6-potassium dioxaoctane sulphonate, and the fluid further contains as oxidation inhibitors pentaerythryl-tetrakis-3-(3',5'-di-tert-butyl-4-hydroxy-phenyl)propionate and alkylated phenyl-alpha-naphthylamine, with the following ratio of starting components, wt %: polybutyl methacrylate 7.0-11.0; epoxy compound 2.0-5.0; 4-trifluoromethylperfluoro-3,6-potassium dioxaoctane sulphonate 0.06-0.14; 2,6-di-tert-butyl-4-methyl-phenol 0.4-1.0; pentaerythryl-tetrakis-3-(3',5'-di-tert-butyl-4-hydroxy-phenyl)propionate 0.25-0.75; alkylated phenyl-alpha-naphthylamine 0.8-1.2; 1,2,3-benzotriazole 0.005-0.015; dye 0.001-0.005; mixture of phosphoric esters - up to 100, with the following ratio of phosphoric esters in the mixture, wt %: tributyl phosphate 70.0-80.0; dibutyl phenyl phosphate 4.0-10.0; triisobutyl phosphate 10.0-20.0; trixylenyl phosphate 4.0-10.0.

EFFECT: high thermal oxidative stability, improved lubricant properties and hydrolytic stability of the working fluid.

3 tbl

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