CN105924344A - High-quality zinc stearate prepared from glyceryl tristearate - Google Patents
High-quality zinc stearate prepared from glyceryl tristearate Download PDFInfo
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- CN105924344A CN105924344A CN201610347360.8A CN201610347360A CN105924344A CN 105924344 A CN105924344 A CN 105924344A CN 201610347360 A CN201610347360 A CN 201610347360A CN 105924344 A CN105924344 A CN 105924344A
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- zinc stearate
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- glyceryl tristearate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C53/00—Saturated compounds having only one carboxyl group bound to an acyclic carbon atom or hydrogen
- C07C53/126—Acids containing more than four carbon atoms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention belongs to the technical field of chemical engineering, and particularly relates to high-quality zinc stearate prepared from glyceryl tristearate. A preparation technology of zinc stearate comprises the following steps that 1, glyceryl tristearate and water are hydrolyzed under the action of a catalyst and an antioxidant; 2, zinc oxide and a catalyst are added stepwise, condensing, dewatering and salt forming are conducted, and zinc stearate is synthesized. Zinc stearate is high in preparation yield, good in color and cluster, low in free acid content and stable in quality, and the related quality indexes meet the related requirements on I type zinc stearate in HG/T3667-2012; in addition, no wastewater containing chlorine and sulfate ions is discharged in the preparation process of zinc stearate, the production process is safe and environmentally friendly, and the total production cost is low. Zinc stearate is high in quality and has the better practicability and comparability compared with similar products on the market in practical application.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of high-quality stearic acid utilizing glyceryl tristearate to prepare
Zinc.
Background technology
Zinc stearate belongs to the one of stearate apoplexy due to endogenous wind, be mainly used as nontoxic polyvinyl chloride stabilizer, the lubricant of cosmetics,
Styrene resin, the releasing agent of hard rubber article, paint flatting agent and rubber industry do the softening agent of sizing material, interleaving agent, should
With quite varied.Along with industrial expansions such as plastics, coating and petrochemical industries, domestic market is to the demand of zinc stearate year by year
Increase.
At present, the commonly used double decomposition of domestic production zinc stearate synthesizes, and its concrete technology is with stearic acid as primary raw material,
With water as medium, carry out saponification by adding sodium hydroxide after stearic acid heating and melting, add zinc salt the most in the reaction product
Aqueous solution carries out metathesis reaction and generates metallic soap precipitation, finally removes by-product with substantial amounts of washing, then through water dumping, the work such as is dried
Skill, obtains zinc stearate finished product.Double decomposition reaction condition is gentle, and the color and luster prepared is good, stability is high, but exists and produce
Efficiency is low, energy consumption and the shortcoming such as water consumption is high.And double decomposition produce discharge during zinc stearate substantial amounts of chloride, sulfate radical from
The waste water of son, causes the biggest pollution to environment;Simultaneously as product metal soap is to generate in surfactant sodium soap solution
, therefore granule is little, dispersion is high, surface adsorption is strong for precipitation, thus causes filter cake moisture content high, and energy consumption for drying is big, product
Apparent density is big, and dust from flying is serious, packaging agent accumulating expense is high.Fusion method is that industrial wide variety of another is hard
The synthetic method of fat acid zinc, its concrete technology is that the temperature that stearic acid and zinc oxide are mixed and heated to more than zinc stearate fusing point is stirred
Mixing reaction, the cooled pulverizing of molten state product or pelletize obtain product.Chinese patent application 201310012047.5 discloses one
Super-thin sheet-shaped zinc stearate, its composition with percentage by weight is: zinc oxide 12%-15%, stearic acid 80%-85%, catalyst
2%-6%, its preparation technology is to be dividedly in some parts zinc oxide and catalyst after stearic acid melts, and has reacted rear fused mass through double rod pressures
Sheet machine cooling compression molding i.e. obtains described super-thin sheet-shaped zinc stearate.It is with short production cycle that fusion method prepares zinc stearate, arranges without waste liquid
Putting, product does not contains other inorganic salt anion, few with water, but the product prepared to there is purity low, free fatty acid content
Height, the problems such as product color is bad.
It is high the most in various degree to there is production cost in the zinc stearate that most domestic zinc stearate manufacturer is produced, production process
Environmental pollution is serious or the zinc stearate for preparing by People's Republic of China's chemical industry standard, " HG/T3667-2012 is stearic
Acid zinc " problem such as detection part index number is the most up to standard, and particularly free acid content is high, its preparation technology and quality still need to change further
Entering, thus limit the application in its at home and abroad market, high-quality zinc stearate mostly relies on import, expensive.
Therefore, study a kind of overall manufacturing low cost, production process safety and environmental protection, zinc stearate that product quality is high have higher warp
Ji benefit and social benefit.
Summary of the invention
It is an object of the invention to overcome existing technological deficiency, it is provided that a kind of utilize that glyceryl tristearate prepares high-quality
Amount zinc stearate.The zinc stearate that the present invention provides, purity is high, and color and luster is good, and free acid content is low, and quality meets
The relevant criterion of I type zinc stearate in HG/T3667-2012, its production process is without chloride, the waste water row of sulfate ion simultaneously
Putting, productivity is high, and energy consumption is low, and total cost of production is low, has more practicality and can in actual applications compared with the like product of market
Compare property.
Technical scheme is as follows:
A kind of high-quality zinc stearate utilizing glyceryl tristearate to prepare, its preparation technology comprises the steps:
S1: take glyceryl tristearate, feeds intake while stir, and temperature is maintained at 80-100 DEG C, treats that glyceryl tristearate is whole
Adding catalyst A, antioxidant and water after Rong Rong, be 120-150 DEG C in temperature, pressure is to enter under conditions of 0.6-0.8MPa
Row hydrolysis, hydrolyzate stands 30-60min, oil-water separation, and oil phase filter pressing is reclaimed catalyst and i.e. obtained stearic acid;
S2: being added in zinc stearate reactor by stearic acid in S1, temperature is maintained at 100-115 DEG C, adds oxidation while stirring
Zinc, after having fed intake, temperature of charge rises to 115-120 DEG C, adds catalyst B, stirring reaction 25-35min;
S3: again add zinc oxide and catalyst B, react under conditions of temperature is 125-135 DEG C, stop stirring, thing
After strand foam is down to equilibrium point, add catalyst B, under conditions of temperature is 145-155 DEG C, reacts 15-25min;
S4: add sodium hydroxide, isothermal reaction 30-40min while stirring;
S5: open vacuum pump, regulation vacuum to-0.09--0.07MPa, dehydration, stably react 50-70min under the conditions of constant temperature and pressure,
Reaction terminating, obtains zinc stearate.
Preferably, described catalyst A is zinc oxide and Al2O3The mixture of-MgO, counts in mass ratio, zinc oxide: Al2O3-MgO
Being 1: 3-8, the consumption of catalyst A is the 2%-6% of glyceryl tristearate quality.Wherein, Al2O3-MgO passes through the sedimentation method
Prepare, ratio, Al2O3: MgO is 1-3: 1.
Preferably, described antioxidant is antioxidant 1076, antioxidant DLTDP and the mixture of antioxidant T501, by quality
Than meter, antioxidant 1076: antioxidant DLTDP: antioxidant T501 is 0.12-0.20: 0.26-0.38: 1, the consumption of antioxidant
0.1%-0.8% for glyceryl tristearate quality.
Preferably, in described step S1, count in mass ratio, glyceryl tristearate: water is 1: 0.4-0.6.
Catalyst B is selected from one or more in peroxide, low carbon fatty acid, it is preferable that selected from hydrogen peroxide, peroxide
Change one or more in sodium, potassium peroxide, calper calcium peroxide, Magnesium dioxide and zinc peroxide.
Preferably, described catalyst B is the mixture of hydrogen peroxide and zinc peroxide, counts in mass ratio, hydrogen peroxide: peroxide
Changing zinc is 2-5: 1.
Preferably, in described step S2, the consumption of zinc oxide is the 8%-10% of glyceryl tristearate quality, catalyst B's
Consumption is the 2%-5% of glyceryl tristearate quality.
Preferably, in described step S3, the consumption of zinc oxide is the 2.4%-4% of glyceryl tristearate quality, catalyst B
The 0.5%-2% that first time addition is glyceryl tristearate quality, the catalyst B addition added is three glycerol stearate
The 0.5%-1% of ester quality.
Preferably, in described step S4, the consumption of sodium hydroxide is the 0.1%-0.3% of glyceryl tristearate quality.
The zinc stearate that the present invention provides, its preparation technology includes that glyceryl tristearate hydrolysis and stearic acid are de-with zinc oxide condensation
Water becomes salt two-step reaction.In glyceryl tristearate hydrolytic process, zinc oxide can weaken ester bond bond energy by adsorption, makes ester
Key is susceptible to hydrolysis, Al2O3-MgO is solid acid alkali catalytic agent, at zinc oxide and Al2O3The catalytic action of-MgO composite catalyst
Under, glyceryl tristearate hydrolysis generates stearic acid and glycerol, and percent hydrolysis reaches more than 96%, and the glycerol that hydrolysis produces is dissolved in
Water separates with stearic acid, is conducive to improving the purity of finished product;And the mixture of isolated glycerol and water is separated and dense
Contracting processes can obtain glycerol, is conducive to improving the availability of raw material.Antioxidant 1076, antioxidant DLTDP and antioxidant T501
Under the conditions of the interpolation of composite antioxidant can avoid pyroreaction, material aoxidizes, it is ensured that finished product colourity.Stearic acid and zinc oxide
Condensation be dehydrated into salt during, using the mixture of hydrogen peroxide and zinc peroxide as composite catalyst do not introduce new impurity component,
Improve the productivity being remarkably improved zinc stearate while product purity, and in reaction system, add a small amount of sodium hydroxide can be notable
Reducing the free acid content in zinc stearate, meanwhile, part of stearic acid and sodium hydroxide react and generate minimal amount of stearic acid
Sodium can play Action of Surfactant in the reaction, improves the effect of reaction, reacts fully and carry out, and improves product yield.
Compared with prior art, the beneficial effects of the present invention is:
1) zinc stearate that the present invention provides, uses glyceryl tristearate and zinc oxide as raw material, and cost of material is low, produces
Process energy consumption is low, and zinc stearate productivity is high, and total cost of production is low;
2) the zinc stearate production process that the present invention provides is without chloride, the discharge of wastewater of sulfate ion, non-dusting situation,
Production process safety and environmental protection;
3) zinc stearate that the present invention provides, purity is high, and color and luster is good, and free acid content is low, and quality meets HG/T3667-2012
The relevant criterion of middle I type zinc stearate.
Detailed description of the invention
Further describe the present invention below by way of detailed description of the invention, but the present invention is not limited only to following example.In the present invention
In the range of or without departing from present disclosure, spirit and scope, the present invention is suitably modified, replaces effect phase
Same component, will become apparent to those skilled in the art that they are considered as being included within the scope of the present invention.
The preparation of embodiment 1 zinc stearate
S1: take glyceryl tristearate, feeds intake while stir, and temperature is maintained at 100 DEG C, treats that glyceryl tristearate all melts
Adding catalyst A, antioxidant and water after melting, be 135 DEG C in temperature, pressure is the reaction that is hydrolyzed under conditions of 0.7MPa,
Hydrolyzate stands 45min, oil-water separation, and oil phase filter pressing is reclaimed catalyst and i.e. obtained stearic acid;
Wherein, count in mass ratio, in catalyst A, zinc oxide: Al2O3-MgO is 1: 6, and its consumption is three glycerol stearate
The 4% of ester quality, Al2O3-MgO is prepared by the sedimentation method, ratio, Al2O3: MgO is 2.5: 1;
Count in mass ratio, in antioxidant, antioxidant 1076: antioxidant DLTDP: antioxidant T501 is 0.12: 0.38: 1,
Its consumption is the 0.5% of glyceryl tristearate quality;
Count in mass ratio, glyceryl tristearate: water is 1: 0.45;
S2: being added in zinc stearate reactor by stearic acid in S1, temperature is maintained at 110 DEG C, adds three stearic acid while stirring
The zinc oxide of glyceride quality 9%, after having fed intake, temperature of charge rises to 120 DEG C, adds glyceryl tristearate quality 3%
Catalyst B, stirring reaction 30min;
Wherein, catalyst B is the mixture of hydrogen peroxide and zinc peroxide, counts in mass ratio, hydrogen peroxide: zinc peroxide is
4∶1;
S3: add zinc oxide and the catalyst B of glyceryl tristearate quality 2% of glyceryl tristearate quality 3.8%,
Temperature is reacted under conditions of being 130 DEG C, stops stirring, after material foam is down to equilibrium point, adds glyceryl tristearate
The catalyst B of quality 0.5%, reacts 20min under conditions of temperature is 150 DEG C;
S4: add the sodium hydroxide of glyceryl tristearate quality 0.25%, isothermal reaction 30min while stirring;
S5: open vacuum pump, regulation vacuum to-0.08MPa, dehydration, stably react 60min under the conditions of constant temperature and pressure, instead
Should terminate, sampling detection, qualified after dust, packaging warehouse-in, obtain zinc stearate, its productivity is 94.87%.
The preparation of embodiment 2 zinc stearate
S1: take glyceryl tristearate, feeds intake while stir, and temperature is maintained at 100 DEG C, treats that glyceryl tristearate all melts
Adding catalyst A, antioxidant and water after melting, be 120 DEG C in temperature, pressure is the reaction that is hydrolyzed under conditions of 0.8MPa,
Hydrolyzate stands 40min, oil-water separation, and oil phase filter pressing is reclaimed catalyst and i.e. obtained stearic acid;
Wherein, count in mass ratio, in catalyst A, zinc oxide: Al2O3-MgO is 1: 4, and its consumption is three glycerol stearate
The 5.5% of ester quality, Al2O3-MgO is prepared by the sedimentation method, ratio, Al2O3: MgO is 2: 1;
Count in mass ratio, in antioxidant, antioxidant 1076: antioxidant DLTDP: antioxidant T501 is 0.15: 0.32: 1,
Its consumption is the 0.3% of glyceryl tristearate quality;
Count in mass ratio, glyceryl tristearate: water is 1: 0.5;
S2: being added in zinc stearate reactor by stearic acid in S1, temperature is maintained at 115 DEG C, adds three stearic acid while stirring
The zinc oxide of glyceride quality 10%, after having fed intake, temperature of charge rises to 120 DEG C, adds glyceryl tristearate quality 4%
Catalyst B, stirring reaction 35min;
Wherein, catalyst B is hydrogen peroxide;
S3: add zinc oxide and the catalyst B of glyceryl tristearate quality 2% of glyceryl tristearate quality 3.4%,
Temperature is reacted under conditions of being 130 DEG C, stops stirring, after material foam is down to equilibrium point, adds glyceryl tristearate
The catalyst B of quality 1%, reacts 25min under conditions of temperature is 150 DEG C;
S4: add the sodium hydroxide of glyceryl tristearate quality 0.2%, isothermal reaction 35min while stirring;
S5: open vacuum pump, regulation vacuum to-0.09MPa, dehydration, stably react 60min under the conditions of constant temperature and pressure, instead
Should terminate, sampling detection, qualified after dust, packaging warehouse-in, obtain zinc stearate, its productivity is 91.68%.
Comparative example 1
In S1, catalyst A is Al2O3-MgO, its consumption is the 6% of glyceryl tristearate quality, Al2O3-MgO passes through
The sedimentation method prepare, ratio, Al2O3: MgO is 2: 1.
Remaining step is with embodiment 1, and zinc stearate productivity is 75.86%.
Comparative example 2
In step S4, without sodium hydroxide, remaining step is with embodiment 1, and zinc stearate productivity is 82.72%.
With reference to People's Republic of China's chemical industry standard " HG/T3667-2012 zinc stearate " to embodiment of the present invention 1-2, right
The zinc stearate of ratio 1-2 synthesis carries out index of correlation detection, and testing result is shown in Table 1.
Table 1 zinc stearate Indexs measure result
From table 1 result of the test, the zinc stearate free acid content of embodiment of the present invention synthesis is low, and quality is significantly better than contrast
The zinc stearate of example synthesis, understand embodiment 1 is preferred embodiment simultaneously.The zinc stearate preparation that the present invention provides is produced
Rate is high, and color and luster is good, and free acid content is low, steady quality, and correlated quality index meets I type stearic acid in HG/T3667-2012
The requirement of zinc, and the zinc stearate preparation process that the present invention provides is without chloride, the discharge of wastewater of sulfate ion, production process peace
Loopful is protected, and total cost of production is low, has more practicality and comparability in actual applications compared with the like product of market.
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert the present invention
Be embodied as be confined to these explanations.For general technical staff of the technical field of the invention, without departing from this
On the premise of inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. the high-quality zinc stearate that a kind utilizes glyceryl tristearate to prepare, it is characterised in that described zinc stearate
Preparation technology comprises the steps:
S1: take glyceryl tristearate, feeds intake while stir, and temperature is maintained at 80-100 DEG C, treats that glyceryl tristearate is whole
Adding catalyst A, antioxidant and water after Rong Rong, be 120-150 DEG C in temperature, pressure is to enter under conditions of 0.6-0.8MPa
Row hydrolysis, hydrolyzate stands 30-60min, oil-water separation, and oil phase filter pressing is reclaimed catalyst and i.e. obtained stearic acid;
S2: being added in zinc stearate reactor by stearic acid in S1, temperature is maintained at 100-115 DEG C, adds oxidation while stirring
Zinc, after having fed intake, temperature of charge rises to 115-120 DEG C, adds catalyst B, stirring reaction 25-35min;
S3: again add zinc oxide and catalyst B, react under conditions of temperature is 125-135 DEG C, stop stirring, thing
After strand foam is down to equilibrium point, add catalyst B, under conditions of temperature is 145-155 DEG C, reacts 15-25min;
S4: add sodium hydroxide, isothermal reaction 30-40min while stirring;
S5: open vacuum pump, regulation vacuum to-0.09--0.07MPa, dehydration, stably react 50-70min under the conditions of constant temperature and pressure,
Reaction terminating, obtains zinc stearate.
High-quality zinc stearate the most according to claim 1, it is characterised in that described catalyst A be zinc oxide and
Al2O3The mixture of-MgO, counts in mass ratio, zinc oxide: Al2O3-MgO is 1: 3-8, and the consumption of catalyst A is three hard
The 2%-6% of glycerol quality.
High-quality zinc stearate the most according to claim 2, it is characterised in that described Al2O3In-MgO, in molar ratio
Meter, Al2O3: MgO is 1-3: 1.
High-quality zinc stearate the most according to claim 1, it is characterised in that described antioxidant be antioxidant 1076,
Antioxidant DLTDP and the mixture of antioxidant T501, count, antioxidant 1076 in mass ratio: antioxidant DLTDP: antioxygen
Agent T501 is 0.12-0.20: 0.26-0.38: 1, and the consumption of antioxidant is the 0.1%-0.8% of glyceryl tristearate quality.
High-quality zinc stearate the most according to claim 1, it is characterised in that in described step S1, count in mass ratio,
Glyceryl tristearate: water is 1: 0.4-0.6.
High-quality zinc stearate the most according to claim 1, it is characterised in that described catalyst B selected from hydrogen peroxide,
One or more in sodium peroxide, potassium peroxide, calper calcium peroxide, Magnesium dioxide and zinc peroxide.
High-quality zinc stearate the most according to claim 6, it is characterised in that described catalyst B is hydrogen peroxide and mistake
The mixture of zinc oxide, counts in mass ratio, hydrogen peroxide: zinc peroxide is 2-5: 1.
High-quality zinc stearate the most according to claim 1, it is characterised in that in described step S2, the consumption of zinc oxide
For the 8%-10% of glyceryl tristearate quality, the consumption of catalyst B is the 2%-5% of glyceryl tristearate quality.
High-quality zinc stearate the most according to claim 1, it is characterised in that in described step S3, the consumption of zinc oxide
First time addition for the 2.4%-4% of glyceryl tristearate quality, catalyst B is glyceryl tristearate quality
0.5%-2%, the 0.5%-1% that catalyst B addition is glyceryl tristearate quality added.
High-quality zinc stearate the most according to claim 1, it is characterised in that in described step S4, sodium hydroxide
Consumption is the 0.1%-0.3% of glyceryl tristearate quality.
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CN112341326A (en) * | 2020-09-30 | 2021-02-09 | 南通新邦化工科技有限公司 | Novel preparation process of zinc stearate |
US11660726B2 (en) | 2019-09-05 | 2023-05-30 | Saint-Gobain Abrasives, Inc. | Coated abrasives having an improved supersize coating |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US11660726B2 (en) | 2019-09-05 | 2023-05-30 | Saint-Gobain Abrasives, Inc. | Coated abrasives having an improved supersize coating |
CN112341326A (en) * | 2020-09-30 | 2021-02-09 | 南通新邦化工科技有限公司 | Novel preparation process of zinc stearate |
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