CN108130156A - A kind of preparation method of modified antimony sulantimonate - Google Patents
A kind of preparation method of modified antimony sulantimonate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/24—Compounds containing phosphorus, arsenic or antimony
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
- C01G30/02—Antimonates; Antimonites
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/02—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2217/028—Macromolecular compounds obtained from nitrogen containing monomers by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a nitrogen-containing hetero ring
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/09—Complexes with metals
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/26—Waterproofing or water resistance
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Abstract
The present invention discloses a kind of preparation method of modified antimony sulantimonate, thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and surfactant solution are added in simultaneously in the complex solution of trivalent antimony and disperseed using ultrasonic wave, the temperature of the reaction system is controlled at 20 35 DEG C, and it is 6.3 8.2 to control the pH value of the reaction system with hydrochloric acid, whole materials are continuing with ultrasonic wave and disperse 10 15min after adding in, filtering, obtains antimony sulantimonate crude product；Then wash antimony sulantimonate crude product 12 times with the potassium sodium tartrate solution of a concentration of 3 7g/L, then with purifying water washing 23 times to get；The present invention is modified antimony sulantimonate surface using polyvinylpyrrolidone and surfactant, allow antimony sulantimonate that there is good hydrophobic performance and oleophylic performance, and particle is nanoscale, its dispersibility and compatibility in basic grease is made to increase significantly, hence it is evident that improve the greasy property of product.
Description
Technical field
The present invention relates to chemical fields, more particularly relate to a kind of preparation method of modified antimony sulantimonate.
Background technology
Antimony sulantimonate is a kind of extreme-pressure anti-wear lubricating grease additive haveing excellent performance, and can significantly improve lubricant grease
Sintering load and load capacity reduce friction coefficient, are widely used in mining machinery, ship and military equipment field.Thio antimony
Sour antimony and all basic fat such as lithium saponify, clay fat, silicone grease and aluminum complex grease etc. have preferable compatibility, to various
Alloy has good lubricant effect including being difficult to the chromium tool steel lubricated and stainless steel etc., and thermal stability is good, is suitable for Gao Zhen
The special circumstances such as sky, high load capacity, radiation use.
Preparing antimony sulantimonate at present, there are mainly three types of methods.First method be using antimony oxide and potassium hydroxide as
Antimony sulantimonate is obtained by the reaction in starting material and schlippe's salt, this method needs a large amount of hydrochloric acid to neutralize, and leads to schlippe's salt point
Solution generates hydrogen sulfide gas and produces sulphur simple substance, causes sulfur content in product higher, corrodes in use by lubriation material,
A large amount of ethyl alcohol washing sulphur need to be consumed, generating hydrogen sulfide deteriorates working condition.Second method is used in ethanol medium
Antimony trihalide and schlippe's salt reaction directly synthesize antimony sulantimonate.Although this method reduces the life of hydrogen sulfide and elemental sulfur
Into, but antimony trihalide easily hydrolyzes, and need to use a large amount of organic solvents, cause waste and the pollution of environment water.The third side
Method is to substitute antimony trihalide using antimony oxide directly to react with schlippe's salt in aqueous solution, and it is less to obtain free sulphur
Antimony sulantimonate, but this method need to carry out in acid condition, schlippe's salt easily hydrolyzes, and yield is caused to decline.
Antimony sulantimonate is needed with that could carry out commercial Application after lubricating uniform, but the hydrophily of antimony sulantimonate compared with
Good, lubricating grease has extremely strong lipophile, good dispersed and compatible in order to which antimony sulantimonate example is made to have in lubricating grease
Property, it needs in the synthesis process to control the granularity of antimony sulantimonate and surface nature, reduces the surface energy of particle, prevent
Particle aggregation improves its dispersion performance in lubricating grease；On the other hand to make particle surface that there is the property of hydrophobic oleophylic, change
It is apt to its compatibility with lubricating grease.The surface of material is modified and granularity control usually adds a certain amount of point in the building-up process later stage
Powder and surfactant, processing method mainly have macromolecule surface cladding, surfactant-modified, coupling agent modified etc..
The size of thioantimonic acid antimony particle and the uniformity coefficient of dispersion are larger to Lubrication Properties, with grain diameter
Reduce, the increase of surface atom percentage, surface defect structure increases, nanometer sulfo antimony acid antimony show unique bulk effect,
Quantum size effect and tunnel-effect make its dispersibility and compatibility in basic grease increase significantly, hence it is evident that improve production
The greasy property of product.Therefore, the shortcomings that so overcoming above-mentioned three kinds of preparation methods, provide one kind can prepare small grain size be modified it is thio
The method of metaantimmonic acid antimony is a problem of those skilled in the art's urgent need to resolve.
Invention content
It is an object of the invention to overcome defect of the existing technology, a kind of preparation side of modified antimony sulantimonate is provided
Method.
To achieve these goals, the technical solution adopted by the present invention is as follows：
The preparation method of the modification antimony sulantimonate of the present invention, includes the following steps：
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and surfactant solution are added in into matching for trivalent antimony simultaneously
Disperseed in polymer solution and using ultrasonic wave, control the temperature of the reaction system at 20-35 DEG C, and control this anti-with hydrochloric acid
The pH value for answering system is 6.3-8.2, and whole materials are continuing with ultrasonic wave dispersion 10-15min after adding in, filtering obtains
Antimony sulantimonate crude product；Then it washs antimony sulantimonate crude product 1-2 times with the potassium sodium tartrate solution of a concentration of 3-7g/L, then uses
Purify water washing 2-3 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, surfactant solution and trivalent antimony complex
The volume ratio of solution is 1-1.05：1.05-1.15：0.1-0.5：0.05-0.3.
Preferably, a concentration of 65-75g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution.
Preferably, a concentration of 65-80g/L of antimony in the complex solution of the trivalent antimony.
Preferably, a concentration of 4-10g/L of the polyvinylpyrrolidonesolution solution.
Preferably, it is cetyl trimethylammonium bromide in the surfactant solution, 18 amino trimethyl chlorine
Change ammonium, Cetyltrimethylammonium bromide, 16 amino trimethyl ammonium chlorides, dodecyl trimethyl ammonium chloride, dodecyl
The solution of any one of trimethylammonium bromide, a concentration of 1-15g/L of surfactant in the surfactant solution.
Preferably, thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and surfactant solution are added in three simultaneously
During the complex solution of valency antimony, the addition speed of control thioantimonic acid sodium solution is 12-18mL/min, and polyvinylpyrrolidone is molten
The addition speed of liquid is 3-6mL/min, and the addition speed of surfactant solution is 4-8mL/min.
Preferably, when being disperseed using ultrasonic wave, the frequency for controlling ultrasonic wave is 50-100kHz, power 100-
200w。
Preferably, the preparation method of the complex solution of the trivalent antimony includes the following steps：
It is added in purified water after multi-hydroxy carboxy acid and sodium chloride are mixed, heats the mixed solution while stirring to 35-65
DEG C, antimony oxide powder is added, is filtered after reacting 15-25min, is taken filtrate, obtain the complex solution of trivalent antimony；It is described
The molar ratio of multi-hydroxy carboxy acid and antimony oxide is 4.5-5.7:1.
Preferably, the multi-hydroxy carboxy acid is any one in tartaric acid, citric acid, oxalic acid.
Preferably, in the complex solution of the trivalent antimony chlorion a concentration of 2.5-3.5mol/L.
The present invention is by adopting the above-described technical solution, have the advantages that：
1st, the present invention during antimony sulantimonate is synthesized, using polyvinylpyrrolidone to antimony sulantimonate surface into
Row cladding, changes its surface nature, improves the stability of antimony sulantimonate, it is made to be difficult in subsequent washing procedure molten
Solution effectively improves the yield of antimony sulantimonate；Secondly, using surfactants such as cetyl trimethylammonium bromides to thio antimony
Sour antimony surface is coated, and lipophilic group is made to be adsorbed in antimony sulantimonate surface, and antimony sulantimonate is allowed to have good hydrophobicity
There can be preferable compatibility with lubricant grease, extreme pressure and antiwear performance and greasy property are good, each as additive with oleophylic performance
Kind performance is far more than requirement of the national standard to extreme pressure grease.
2nd, the present invention carries out ultrasonic disperse using ultrasonic wave to the complex solution of trivalent antimony, is conducive to improve thioantimonic acid
Dispersed homogeneous degree of the sodium solution in the complex solution of trivalent antimony promotes the synthetic reaction of antimony sulantimonate, thio to preventing
The reunion of metaantimmonic acid antimony crystal has certain effect, can also improve the uniformity of crystal grain, reduce the grain size of crystal grain, make crystal
The grain size of particle reaches nanoscale, shows unique bulk effect, quantum size effect and tunnel-effect, makes it in base oil
The dispersibility and compatibility of fat increase significantly, hence it is evident that improve the greasy property of product, reduce the usage amount of lubricant grease, have
Good economic benefit and social benefit.
3rd, the present invention is reacted with multi-hydroxy carboxy acid and antimony oxide in sodium chloride solution, obtained trivalent antimony
Complex solution is all more stable in acid, neutral, alkaline system；The sodium chloride of addition is remarkably improved multi-hydroxy carboxy acid couple
The leaching rate of antimony oxide improves raw material availability, reduces production cost.
4th, the present invention is in the preparation process of modified antimony sulantimonate, and the pH value for controlling reaction system is 6.3-8.2, at this
With the complex solution of thioantimonic acid sodium solution and trivalent antimony synthesis antimony sulantimonate in the range of pH, it is suppressed that schlippe's salt
It decomposes, products obtained therefrom performance is good, high purity, and yield is high, suitable for industrialized production, has a good application prospect.
5th, the present invention washs antimony sulantimonate crude product using potassium sodium tartrate solution and purified water, can inhibit wash water
The raising of pH reduces loss of the antimony sulantimonate in washing process, improves antimony sulantimonate finished product yield.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, preferred embodiment is enumerated below, to this hair
Bright further description.However, it is necessary to illustrate, many details listed in specification are used for the purpose of making reader to this
There are one thorough explanations for the one or more aspects of invention, can also realize the present invention's even without these specific details
These aspects.
Embodiment 1
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 18 amino trimethyl ammonia chloride ammonium salt solutions are added in simultaneously
In the tartaric acid complex solution of trivalent antimony and frequency of use is 50kHz, and power is that the ultrasonic wave of 100w is disperseed, and control should
The temperature of reaction system is at 20 DEG C, and it is 6.3 to control the pH value of the reaction system with hydrochloric acid, and whole materials continue after adding in
Disperse 10min using ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then with the potassium sodium tartrate solution of a concentration of 3g/L
Wash antimony sulantimonate crude product 2 times, then with purify water washing 3 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, 18 amino trimethyl ammonia chloride ammonium salt solutions and trivalent
The volume ratio of the tartaric acid complex solution of antimony is 1：1.05：0.1：0.05；
A concentration of 65g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the tartaric acid complex solution of trivalent antimony
The amino trimethyl ammonia chloride ammonium salt solution of a concentration of 65g/L of antimony, a concentration of 4g/L of polyvinylpyrrolidonesolution solution, 18 concentration
For 1g/L.
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 18 amino trimethyl ammonia chloride ammonium salt solutions are added in simultaneously
During the tartaric acid complex solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 12mL/min, polyvinyl pyrrole
The addition speed of alkanone solution is 3mL/min, and the addition speed of 18 amino trimethyl ammonia chloride ammonium salt solutions is 4mL/min.
The preparation method of the tartaric acid complex solution of the trivalent antimony includes the following steps：
It is added in purified water after tartaric acid and sodium chloride are mixed, heats the mixed solution while stirring to 35 DEG C, then added
Enter antimony oxide powder, filtered after reacting 15min, take filtrate, obtain the tartaric acid complex solution of trivalent antimony；The winestone
The molar ratio of acid and antimony oxide is 4.5:1, a concentration of 2.5mol/L of the Chlorine in Solution ion.
Embodiment 2
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and cetyl trimethylammonium bromide solution are added in simultaneously
In the citric acid compound solution of trivalent antimony and frequency of use is 60kHz, and power is that the ultrasonic wave of 120w is disperseed, and control should
The temperature of reaction system is at 23 DEG C, and it is 6.6 to control the pH value of the reaction system with hydrochloric acid, and whole materials continue after adding in
Disperse 11min using ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then with the potassium sodium tartrate solution of a concentration of 4g/L
Wash antimony sulantimonate crude product 2 times, then with purify water washing 2 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, cetyl trimethylammonium bromide solution and trivalent
The volume ratio of the citric acid compound solution of antimony is 1.01：1.07：0.2：0.1；
A concentration of 68g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the citric acid compound solution of trivalent antimony
A concentration of 69g/L of antimony, a concentration of 5g/L of polyvinylpyrrolidonesolution solution, the concentration of cetyl trimethylammonium bromide solution
For 5g/L.
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and cetyl trimethylammonium bromide solution are added in simultaneously
During the citric acid compound solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 14mL/min, polyvinyl pyrrole
The addition speed of alkanone solution is 4mL/min, and the addition speed of cetyl trimethylammonium bromide solution is 5mL/min.
The preparation method of the citric acid compound solution of the trivalent antimony includes the following steps：
It is added in purified water after citric acid and sodium chloride are mixed, heats the mixed solution while stirring to 42 DEG C, then added
Enter antimony oxide powder, filtered after reacting 18min, take filtrate, obtain the citric acid compound solution of trivalent antimony；The lemon
The molar ratio of acid and antimony oxide is 4.8:1, a concentration of 2.7mol/L of the Chlorine in Solution ion.
Embodiment 3
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 18 amino trimethyl ammonia chloride ammonium salt solutions are added in simultaneously
In the Oxalate Complexes solution of trivalent antimony and frequency of use is 70kHz, and power is that the ultrasonic wave of 140w is disperseed, and controls this anti-
The temperature of system is answered at 28 DEG C, and it is 7.0 to control the pH value of the reaction system with hydrochloric acid, whole materials continue to make after adding in
Disperse 12min with ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then it is washed with the potassium sodium tartrate solution of a concentration of 5g/L
Wash antimony sulantimonate crude product 1 time, then with purifying water washing 3 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, 18 amino trimethyl ammonia chloride ammonium salt solutions and trivalent
The volume ratio of the Oxalate Complexes solution of antimony is 1.02：1.1：0.3：0.18；
A concentration of 70g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the Oxalate Complexes solution of trivalent antimony
A concentration of 73g/L of antimony, a concentration of 5g/L of polyvinylpyrrolidonesolution solution, 18 amino trimethyl ammonia chloride ammonium salt solutions it is a concentration of
7g/L。
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 18 amino trimethyl ammonia chloride ammonium salt solutions are added in simultaneously
During the Oxalate Complexes solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 16mL/min, polyvinylpyrrolidine
The addition speed of ketone solution is 5mL/min, and the addition speed of 18 amino trimethyl ammonia chloride ammonium salt solutions is 6mL/min.
The preparation method of the Oxalate Complexes solution of the trivalent antimony includes the following steps：
It is added in purified water after oxalic acid and sodium chloride are mixed, heats the mixed solution while stirring to 50 DEG C, add
Antimony oxide powder filters after reacting 20min, takes filtrate, obtain the Oxalate Complexes solution of trivalent antimony；The oxalic acid and three
The molar ratio for aoxidizing two antimony is 5.1:1, a concentration of 3mol/L of the Chlorine in Solution ion.
Embodiment 4
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 16 amino trimethyl ammonia chloride ammonium salt solutions are added in simultaneously
In the tartaric acid complex solution of trivalent antimony and frequency of use is 80kHz, and power is that the ultrasonic wave of 160w is disperseed, and control should
The temperature of reaction system is at 30 DEG C, and it is 7.4 to control the pH value of the reaction system with hydrochloric acid, and whole materials continue after adding in
Disperse 13min using ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then with the potassium sodium tartrate solution of a concentration of 6g/L
Wash antimony sulantimonate crude product 2 times, then with purify water washing 2 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, 16 amino trimethyl ammonia chloride ammonium salt solutions and trivalent
The volume ratio of the tartaric acid complex solution of antimony is 1.03：1.12：0.4：0.23；
A concentration of 72g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the tartaric acid complex solution of trivalent antimony
The amino trimethyl ammonia chloride ammonium salt solution of a concentration of 75g/L of antimony, a concentration of 7g/L of polyvinylpyrrolidonesolution solution, 16 concentration
For 9g/L.
By thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and 16 amino trimethyl ammonium chloride Solutions Solutions simultaneously
When adding in the tartaric acid complex solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 17mL/min, polyethylene
The addition speed of pyrrolidone solution is 6mL/min, and the addition speed of 16 amino trimethyl ammonia chloride ammonium salt solutions is 7mL/min.
The preparation method of the tartaric acid complex solution of the trivalent antimony includes the following steps：
It is added in purified water after tartaric acid and sodium chloride are mixed, heats the mixed solution while stirring to 55 DEG C, then added
Enter antimony oxide powder, filtered after reacting 24min, take filtrate, obtain the tartaric acid complex solution of trivalent antimony；The winestone
The molar ratio of acid and antimony oxide is 5.3:1, a concentration of 3.2mol/L of the Chlorine in Solution ion.
Embodiment 5
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and dodecyl trimethyl ammonium chloride solution are added in simultaneously
In the citric acid compound solution of trivalent antimony and frequency of use is 90kHz, and power is that the ultrasonic wave of 180w is disperseed, and control should
The temperature of reaction system is at 33 DEG C, and it is 7.8 to control the pH value of the reaction system with hydrochloric acid, and whole materials continue after adding in
Disperse 14min using ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then with the potassium sodium tartrate solution of a concentration of 7g/L
Wash antimony sulantimonate crude product 1 time, then with purify water washing 2 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, dodecyl trimethyl ammonium chloride solution and trivalent
The volume ratio of the citric acid compound solution of antimony is 1.04：1.14：0.5：0.27；
A concentration of 74g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the citric acid compound solution of trivalent antimony
A concentration of 77g/L of antimony, a concentration of 8g/L of polyvinylpyrrolidonesolution solution, the concentration of dodecyl trimethyl ammonium chloride solution
For 12g/L.
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and dodecyl trimethyl ammonium chloride solution are added in simultaneously
During the citric acid compound solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 18mL/min, polyvinyl pyrrole
The addition speed of alkanone solution is 5mL/min, and the addition speed of dodecyl trimethyl ammonium chloride solution is 8mL/min.
The preparation method of the citric acid compound solution of the trivalent antimony includes the following steps：
It is added in purified water after citric acid and sodium chloride are mixed, heats the mixed solution while stirring to 60 DEG C, then added
Enter antimony oxide powder, filtered after reacting 25min, take filtrate, obtain the citric acid compound solution of trivalent antimony；The lemon
The molar ratio of acid and antimony oxide is 5.5:1, a concentration of 3.4mol/L of the Chlorine in Solution ion.
Embodiment 6
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and dodecyl trimethyl ammonium bromide solution are added in simultaneously
In the Oxalate Complexes solution of trivalent antimony and frequency of use is 100kHz, and power is that the ultrasonic wave of 200w is disperseed, and control should
The temperature of reaction system is at 35 DEG C, and it is 8.4 to control the pH value of the reaction system with hydrochloric acid, and whole materials continue after adding in
Disperse 15min using ultrasonic wave, filtering obtains antimony sulantimonate crude product；Then with the potassium sodium tartrate solution of a concentration of 5g/L
Wash antimony sulantimonate crude product 2 times, then with purify water washing 3 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, dodecyl trimethyl ammonium bromide solution and trivalent
The volume ratio of the Oxalate Complexes solution of antimony is 1.05：1.15：0.4：0.3；
A concentration of 75g/L of a concentration of antimony of antimony in the thioantimonic acid sodium solution, in the Oxalate Complexes solution of trivalent antimony
A concentration of 80g/L of antimony, a concentration of 10g/L of polyvinylpyrrolidonesolution solution, the concentration of dodecyl trimethyl ammonium bromide solution
For 15g/L.
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and dodecyl trimethyl ammonium bromide solution are added in simultaneously
During the Oxalate Complexes solution of trivalent antimony, the addition speed of control thioantimonic acid sodium solution is 15mL/min, polyvinylpyrrolidine
The addition speed of ketone solution is 6mL/min, and the addition speed of dodecyl trimethyl ammonium bromide solution is 7mL/min.
The preparation method of the Oxalate Complexes solution of the trivalent antimony includes the following steps：
It is added in purified water after oxalic acid and sodium chloride are mixed, heats the mixed solution while stirring to 65 DEG C, add
Antimony oxide powder filters after reacting 25min, takes filtrate, obtain the Oxalate Complexes solution of trivalent antimony；The oxalic acid and three
The molar ratio for aoxidizing two antimony is 5.7:1, a concentration of 3.5mol/L of the Chlorine in Solution ion.
Claims (10)
1. a kind of preparation method of modified antimony sulantimonate, which is characterized in that include the following steps：
Thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution and surfactant solution are added in the complex of trivalent antimony simultaneously
Disperseed in solution and using ultrasonic wave, control the temperature of the reaction system at 20-35 DEG C, and the reactant is controlled with hydrochloric acid
The pH value of system is 6.3-8.2, and whole materials are continuing with ultrasonic wave dispersion 10-15min after adding in, filtering obtains thio
Metaantimmonic acid antimony crude product；Then wash antimony sulantimonate crude product 1-2 times with the potassium sodium tartrate solution of a concentration of 3-7g/L, then with purifying
Water washing 2-3 times to get；
The thioantimonic acid sodium solution, polyvinylpyrrolidonesolution solution, surfactant solution and trivalent antimony complex solution
Volume ratio be 1-1.05：1.05-1.15：0.1-0.5：0.05-0.3.
2. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：The schlippe's salt
A concentration of 65-75g/L of a concentration of antimony of antimony in solution.
3. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：The trivalent antimony is matched
A concentration of 65-80g/L of antimony in polymer solution.
4. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：The polyvinyl pyrrole
A concentration of 4-10g/L of alkanone solution.
5. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：The surfactant
It is cetyl trimethylammonium bromide in solution, 18 amino trimethyl ammonium chlorides, Cetyltrimethylammonium bromide, 16 ammonia
The solution of any one of base trimethyl ammonium chloride, dodecyl trimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, it is described
A concentration of 1-15g/L of surfactant in surfactant solution.
6. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：Schlippe's salt is molten
When liquid, polyvinylpyrrolidonesolution solution and surfactant solution add in the complex solution of trivalent antimony simultaneously, thio antimony is controlled
The addition speed of acid sodium solution is 12-18mL/min, and the addition speed of polyvinylpyrrolidonesolution solution is 3-6mL/min, surface
The addition speed of activator solution is 4-8mL/min.
7. the preparation method of modified antimony sulantimonate according to claim 1, it is characterised in that：Divided using ultrasonic wave
When dissipating, the frequency for controlling ultrasonic wave is 50-100kHz, power 100-200w.
8. the preparation method of modified antimony sulantimonate according to claim 1, which is characterized in that the trivalent antimony is matched
The preparation method of polymer solution includes the following steps：
It is added in purified water after multi-hydroxy carboxy acid and sodium chloride are mixed, heats the mixed solution while stirring to 35-65 DEG C, then
Antimony oxide powder is added in, is filtered after reacting 15-25min, is taken filtrate, obtain the complex solution of trivalent antimony；The polyhydroxy
The molar ratio of yl carboxylic acid and antimony oxide is 4.5-5.7:1.
9. the preparation method of modified antimony sulantimonate according to claim 8, it is characterised in that：The multi-hydroxy carboxy acid
For any one in tartaric acid, citric acid, oxalic acid.
10. the preparation method of modified antimony sulantimonate according to claim 8, it is characterised in that：The trivalent antimony
A concentration of 2.5-3.5mol/L of chlorion in complex solution.
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Citations (4)
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|---|---|---|---|---|
| US4557839A (en) * | 1984-12-21 | 1985-12-10 | Pennwalt Corporation | Synergistic lubricant additives of antimony thioantimonate and molybdenum disulfide or graphite |
| US4735790A (en) * | 1986-12-02 | 1988-04-05 | Pennwalt Corporation | Antimony thioantimonate lubricant additive and preparation |
| CN102583534A (en) * | 2012-02-28 | 2012-07-18 | 益阳生力材料科技有限公司 | Method for preparing nanometer sulfo antimony acid antimony |
| CN103214035A (en) * | 2013-04-11 | 2013-07-24 | 湖南益阳生力材料科技有限公司 | Method for preparing antimony thioantimonate based on stable reaction system |
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2017
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| US4557839A (en) * | 1984-12-21 | 1985-12-10 | Pennwalt Corporation | Synergistic lubricant additives of antimony thioantimonate and molybdenum disulfide or graphite |
| US4735790A (en) * | 1986-12-02 | 1988-04-05 | Pennwalt Corporation | Antimony thioantimonate lubricant additive and preparation |
| CN102583534A (en) * | 2012-02-28 | 2012-07-18 | 益阳生力材料科技有限公司 | Method for preparing nanometer sulfo antimony acid antimony |
| CN103214035A (en) * | 2013-04-11 | 2013-07-24 | 湖南益阳生力材料科技有限公司 | Method for preparing antimony thioantimonate based on stable reaction system |
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