CN105254487A - Environment-friendly metal carboxylate and preparation method thereof - Google Patents
Environment-friendly metal carboxylate and preparation method thereof Download PDFInfo
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- CN105254487A CN105254487A CN201510725800.4A CN201510725800A CN105254487A CN 105254487 A CN105254487 A CN 105254487A CN 201510725800 A CN201510725800 A CN 201510725800A CN 105254487 A CN105254487 A CN 105254487A
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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
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Abstract
The invention discloses an environment-friendly metal carboxylate and a preparation method thereof. The metal carboxylate has the following structure: CH3(CH2)nCOO-M-OOC(CH2)nCH3, wherein M is Zn<2+> and Mg<2+>, and n is equal to 10 to 16. Straight-chain saturated monocarboxylic acid and oxide powder or hydroxide powder of zinc and magnesium are subjected to salt-forming reaction under the action of catalyst, the metal carboxylate is a meltable solid, and after grinding, a powdery environment-friendly metal carboxylate product can be prepared. The preparation process is simple, operability is high, energy is saved, the product purity is high, and the environment-friendly metal carboxylate is environment-friendly, and meets the requirement of ROHS directive, EU (European Union) REACH regulation and EN71-3 standard.
Description
Technical field
The present invention relates to a kind of environment-friendly metal carboxylate salt, the invention still further relates to a kind of preparation method of this metal carboxylate.
Background technology
The preparation method of current straight chain aliphatic saturated monocarboxylic acid metal-salt has four kinds, traditional double decomposition, metathesis single stage method, semi-melting method, direct method.
Tradition double decomposition is also known as two-step approach, and whole reaction is carried out in aqueous phase, is commonly called as WATER-WASHING METHOD or wet method.First in the aliphatic carboxylic acid of melting, add NaOH reactant aqueous solution generate sodium soap (water-soluble), and then replace sodium ion with inorganic metal ion, obtain finished product through centrifugal drying.
Metathesis single stage method improves on traditional double decomposition Process ba-sis, and reaction does not need to carry out replacing and under the prerequisite of water as medium, the aliphatic carboxylic acid of melting directly and metal oxide or oxyhydroxide react again through dehydrating obtained finished product;
Semi-melting method, at the aliphatic carboxylic acid of melting and metal oxide or the temperature of oxyhydroxide below the melting point of generated metal carboxylate, is carried out reacting and directly obtain solid articles in semi-melting state;
Under the direct method condition that to be the aliphatic carboxylic acid of powdery and metal oxide or oxyhydroxide stir in high speed dispersion, directly form powdery solid product.
Produce a large amount of brine wastes in double decomposition production process, environmental pollution is comparatively large, and product is impure more, is eliminated just gradually.
Although metathesis single stage method is carried out improving to traditional technology and improved, all very large to the consumption of the baking needed electric energy of product and water resources in production process, be a kind of waste to resource itself, production process very complicated, production cost is higher.Semi-melting method and direct method are for higher calcium, magnesium metal oxide or the oxyhydroxide of activity, reaction can be carried out, but because temperature of reaction is lower, be difficult to fully and completely react, particularly substantially do not react with aliphatic carboxylic acid under zinc oxide low temperature, these two kinds of techniques lack feasibility in actually operating.
So it is simple to seek a kind of technique, reaction conditions is gentle, workable, the commercial run of preparing metal carboxylate efficiently, is the demand of current industry member.
Summary of the invention
The object of the invention is, in order to overcome weak point of the prior art, to provide a kind of metal carboxylate;
Another object of the present invention is to provide a kind of method preparing this metal carboxylate, and the method technique is relatively simple, and reaction conditions is gentle, workable, and efficiently.
In order to achieve the above object, the present invention adopts following scheme:
A kind of metal carboxylate, is characterized in that having following chemical formula composition:
CH
3(CH
2)
nCOO-M-OOC(CH
2)
nCH
3，
Wherein M is Zn
2+or Mg
2+, n=10 ~ 16.
A kind of metal carboxylate as above, is characterized in that this metal carboxylate is melting solid, is white powder after grinding.
A kind of metal carboxylate as above, is characterized in that described Zn
2+for oxide compound or the oxyhydroxide of zinc.
A kind of metal carboxylate as above, is characterized in that described Mg
2+for oxide compound or the oxyhydroxide of magnesium.
The present invention prepares the method for metal carboxylate as above, and its feature comprises the following steps:
A, by homologous straight chain single fatty acids at 90 ~ 100 DEG C of heating and meltings, be then warming up to 130 ~ 135 DEG C and add Zn
2+or Mg
2+powder, stir about 0.5 hour, mixes; Wherein saturated monocarboxylic acid and Zn
2+or Mg
2+mass ratio is 6.6 ~ 8: 1;
B, the system obtained to steps A add catalyzer, and react 1 ~ 2 hour at 135 ~ 145 DEG C, then cool, pulverize, grind obtained metal carboxylate, wherein said described catalyst levels is monocarboxylic acid and Zn
2+or Mg
2+quality and 2 ~ 5%.
The preparation method of metal carboxylate described above, is characterized in that described homologous straight chain single fatty acids is C
12~ C
18long chained fatty carboxylic acid.If carbon number is less than 12, with metal oxide or oxyhydroxide, especially too fast with metal hydroxides speed of response, cause preparation process to carry out smoothly; If carbon number is greater than 18, then because reactive behavior is too low, and need to add too much catalyzer and auxiliary agent, finally affect purity, the color and luster of product, or even use properties.
The preparation method of metal carboxylate described above, is characterized in that described catalyzer is organic acid, the one in organic dibasic acid or hydrogen peroxide.
The preparation method of metal carboxylate as above, is characterized in that described organic acid is one or more the mixture in formic acid, acetic acid, propionic acid, tosic acid.
The preparation method of metal carboxylate as above, is characterized in that described organic dibasic acid is oxalic acid, propanedioic acid, succinic acid, one or more the mixture in phthalic acid, terephthalic acid.
If consider the catalytic effect of reaction in the present invention, organic dibasic acid and tosic acid can be selected; If consider the purity of final final product, hydrogen peroxide is selected to be advisable; Comprehensive assessment reactive behavior and the feature of environmental protection, choose with hydrogen peroxide and acetic acid proper.Catalyst levels be monocarboxylic acid and zinc, the oxide compound of magnesium or oxyhydroxide quality and 2 ~ 5%.If catalyst levels is less than 2%, reactive behavior is too low, and speed of response is slow, causes preparation process to carry out smoothly; If catalyst levels is greater than 5%, then because speed of response is too fast, reaction is difficult to control, and adds the purity that too much catalyzer finally affects product.
The preparation method of metal carboxylate as above, is characterized in that described Zn
2+or Mg
2+for the zinc of powdery, the oxide compound of magnesium or oxyhydroxide, its size distribution is 2 ~ 50 microns.If particle diameter is less than 2 microns, when disperseing in the fatty carboxylic of melting, easily produces aggregate, carry a large amount of air, hinder the abundant contact of two phase materials, the thoroughness of reaction is affected; If particle diameter is greater than 50 microns, corresponding contact area obviously reduces, and solid-liquid phase is reacted and is difficult to thoroughly carry out, the add-on of metal oxide or oxyhydroxide can only be made obviously to be more than or equal to equivalence ratio, the value of free acid just can be made to drop in qualified scope, finally can have influence on the quality of product.
The zinc used in this programme in addition, the oxide compound of magnesium or oxyhydroxide must meet environmental requirement, content of heavy metal lead: < 50ppm; Cadmium content: < 10ppm.
Reaction in this programme can be carried out in wide temperature range, but temperature of reaction is too low or too highly all can affect quality product.The temperature of reaction of the long chained fatty carboxylic acid of melting and metal oxide or hydroxide powder must higher than resultant metal carboxylate fusing point 10 ~ 20 DEG C, can not too high can not be too low.Because when temperature is too high, whole reaction system bad stability, product can go bad because of high temperature oxidation, yellowish, and hardness increases, and is unfavorable for follow-up grinding and processing; If temperature is too low, reactive behavior reduce, speed of response slows down, for reaction itself do not have what meaning and also reaction time elongated, product colour deepen.In this programme, the reaction times controlled at 1 ~ 2 hour.
The pulverizer used in this programme can adopt the mechanical disintegration of high velocity impact formula, also can adopt comminution by gas stream; Product cut size scope is adjustable, 25 ~ 75 microns (according to client's actual requirement).In crushing process, product removes moisture further.(Zinic stearas: chemical industry standard HG/T3667-2000, weight loss on heating≤0.8%; Magnesium Stearate: pharmacopeia 2005 editions, weight loss on heating≤5.0%).
In sum, beneficial effect of the present invention:
(1) product of the present invention is mainly used in coating, plastics, makeup, powder metallurgy, pharmaceutical industry etc. and does the fields such as the transparent polishing agent of furniture priming paint, plastic heat stabilizer and lubricant, makeup lubricant, powder metallurgy releasing agent and tablet excipient, is a kind of product of environmental type.
(2) this metal carboxylate preparation process is simple, workable, is suitable for the salt-forming reaction of multiple carboxylic acid and metal oxide or hydroxide powder.
(3) temperature of reaction is relatively high, is easy to metal carboxylate product dehydrate, and what quality product was produced compared with traditional technology is significantly improved.
(4) in preparation process, observable index traditional technology has and significantly reduces, and environmental pollution is less, environmental protection.
(5) be solid-state after this metal carboxylate melting cooling, be easy to be processed into powdery finished product; Processing units is easily sought, and is applicable to industrialization and produces.
Embodiment
In order to understand the present invention better, below in conjunction with specific embodiment, the invention will be further described, but the present invention's scope required for protection is not limited to the scope described in embodiment.
The preparation of embodiment 1 Zinic stearas
By the stearic acid (acid number 210) of 900kg at 90 DEG C of heating and meltings, then after being heated to 135 DEG C, adding 135kg zinc oxide (>=99.7%), mix, being uniformly dispersed, in half an hour, divide the hydrogen peroxide catalyzed reaction adding 25kg30% for three times, be incubated 1.5 hours.Then be cooled to solid sheet, obtained Zinic stearas product pulverized by the pulverizer through high velocity impact formula.Its quality index is: Zn content 10.8%; Weight loss on heating≤0.8%; Fusing point >=119 DEG C; Free acid≤0.8%; Fineness≤75 μm.
The preparation of embodiment 2 Zinic stearas
By the stearic acid (acid number 210) of 900kg, at 95 DEG C of heating and meltings, be then heated to 135 DEG C, add 146kg zinc hydroxide (>=99.7%), mixing, be uniformly dispersed after, in half an hour, point to add the hydrogen peroxide catalyzed reaction of 20kg30% for three times, be incubated 1.5 hours.Then be cooled to solid sheet, obtained Zinic stearas product pulverized by the pulverizer through high velocity impact formula.Its quality index is: Zn content 10.6%; Weight loss on heating≤0.8%; Fusing point >=119 DEG C; Free acid≤0.8%; Fineness≤75 μm.
The preparation of embodiment 3 Magnesium Stearate
By the stearic acid (acid number 210) of 900kg, at 100 DEG C of heating and meltings, then 138 DEG C are heated to, add 101.8kg magnesium hydroxide (>=96.0%), mixing, be uniformly dispersed after, in half an hour, divide the hydrogen peroxide catalyzed reaction adding 20kg30% for three times, be incubated 1.5 hours.Then be cooled to solid, obtained magnesium stearate product pulverized by the pulverizer through high velocity impact formula.Its quality index is: Mg content 4.8%; Weight loss on heating≤1.5%; Fusing point >=120 DEG C; Free acid≤2.0%; Fineness≤75 μm.
The preparation of embodiment 4 Magnesium Stearate
By the stearic acid (acid number 210) of 900kg, at 98 DEG C of heating and meltings, be then heated to 138 DEG C, add 98.6kg magnesium oxide (>=96.0%), mixing, be uniformly dispersed after, in half an hour, point to add the hydrogen peroxide catalyzed reaction of 20kg30% for three times, be incubated 1.5 hours.Then be cooled to solid, obtained magnesium stearate product pulverized by the pulverizer through high velocity impact formula.Its quality index is: Mg content 4.8%; Weight loss on heating≤1.5%; Fusing point >=120 DEG C; Free acid≤2.0%; Fineness≤75 μm.
The stearic acid (acid number 210) wherein used in embodiment 1 to 4 is the mixing acid containing the Palmitic acid of 60% and 18 carbonic acid of 40%.
The preparation method of embodiment 5 zinc laurate
After 900kg lauric acid (acid number 280) being heated to 135 DEG C, adding 183.5kg zinc oxide (>=99.7%), mix, being uniformly dispersed, in half an hour, point to add the hydrogen peroxide catalyzed reaction of 20kg30% for three times, be incubated 1.5 hours.Then be cooled to solid sheet, obtained Zinic stearas product pulverized by the pulverizer through high velocity impact formula.Its quality index is: Zn content 14.8%; Weight loss on heating≤0.8%; Fusing point >=124 DEG C; Free acid≤0.8%; Fineness≤75 μm.
Lauric acid (acid number 280) content >=99% wherein used in the present embodiment.
Subordinate list: HG/T3667-2000 Zinic stearas industry standard and pharmacopeia 2005 editions in Magnesium Stearate quality index:
Table 1 Zinic stearas
Table 2 Magnesium Stearate
Claims (10)
1. an environment-friendly metal carboxylate salt, is characterized in that having following chemical formula composition:
CH
3(CH
2)
nCOO-M-OOC(CH
2)
nCH
3，
Wherein M is Zn
2+or Mg
2+, n=10 ~ 16.
2. a kind of environment-friendly metal carboxylate salt according to claim 1, is characterized in that this metal carboxylate is melting solid, is white powder after grinding.
3. a kind of environment-friendly metal carboxylate salt according to claim 1, is characterized in that described Zn
2+for oxide compound or the oxyhydroxide of zinc.
4. a kind of environment-friendly metal carboxylate salt according to claim 1, is characterized in that described Mg
2+for oxide compound or the oxyhydroxide of magnesium.
5. prepare a method for environment-friendly metal carboxylate salt according to claim 1, its feature comprises the following steps:
A, by homologous straight chain single fatty acids at 90 ~ 100 DEG C of heating and meltings, be then warming up to 130 ~ 135 DEG C and add Zn
2+or Mg
2+powder, stir about 0.5 hour, mixes; Wherein saturated monocarboxylic acid and Zn
2+or Mg
2+mass ratio is 6.6 ~ 8: 1;
B, the system obtained to steps A add catalyzer, and react 1 ~ 2 hour at 135 ~ 145 DEG C, then cool, pulverize, grind obtained metal carboxylate, wherein said described catalyst levels is monocarboxylic acid and Zn
2+or Mg
2+quality and 2 ~ 5%.
6. the preparation method of environment-friendly metal carboxylate salt according to claim 5, is characterized in that described homologous straight chain single fatty acids is C
12~ C
18long chained fatty carboxylic acid.
7. the preparation method of environment-friendly metal carboxylate salt according to claim 5, is characterized in that described catalyzer is organic acid, the one in organic dibasic acid or hydrogen peroxide.
8. the preparation method of environment-friendly metal carboxylate salt according to claim 7, is characterized in that described organic acid is one or more the mixture in formic acid, acetic acid, propionic acid, tosic acid.
9. the preparation method of environment-friendly metal carboxylate salt according to claim 7, is characterized in that described organic dibasic acid is oxalic acid, propanedioic acid, succinic acid, one or more the mixture in phthalic acid, terephthalic acid.
10. the preparation method of environment-friendly metal carboxylate salt according to claim 5, is characterized in that described Zn
2+or Mg
2+size distribution be 2 ~ 50 microns, Zn
2+or Mg
2+content of heavy metal lead in powder: < 50ppm; Cadmium content: < 10ppm.
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|---|---|---|---|
| CN201510725800.4A CN105254487A (en) | 2015-10-23 | 2015-10-23 | Environment-friendly metal carboxylate and preparation method thereof |
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ID=55094487
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183324A (en) * | 2019-06-11 | 2019-08-30 | 东莞市汉维科技股份有限公司 | A kind of preparation process of stearate |
| CN110204435A (en) * | 2019-06-11 | 2019-09-06 | 东莞市汉维科技股份有限公司 | A kind of preparation process of stearate |
| CN110386871A (en) * | 2019-08-27 | 2019-10-29 | 如皋市涤诺皂业有限公司 | A kind of production technology of magnesium stearate |
| CN111606799A (en) * | 2020-07-02 | 2020-09-01 | 中山华明泰科技股份有限公司 | Preparation method and application of medicinal composite vegetable fatty acid magnesium |
-
2015
- 2015-10-23 CN CN201510725800.4A patent/CN105254487A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110183324A (en) * | 2019-06-11 | 2019-08-30 | 东莞市汉维科技股份有限公司 | A kind of preparation process of stearate |
| CN110204435A (en) * | 2019-06-11 | 2019-09-06 | 东莞市汉维科技股份有限公司 | A kind of preparation process of stearate |
| CN110183324B (en) * | 2019-06-11 | 2021-09-21 | 东莞市汉维科技股份有限公司 | Preparation process of stearate |
| CN110386871A (en) * | 2019-08-27 | 2019-10-29 | 如皋市涤诺皂业有限公司 | A kind of production technology of magnesium stearate |
| CN111606799A (en) * | 2020-07-02 | 2020-09-01 | 中山华明泰科技股份有限公司 | Preparation method and application of medicinal composite vegetable fatty acid magnesium |
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