CN103588630A - Environmental-protection type copper stearate synthesis method - Google Patents

Environmental-protection type copper stearate synthesis method Download PDF

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Publication number
CN103588630A
CN103588630A CN201310624295.5A CN201310624295A CN103588630A CN 103588630 A CN103588630 A CN 103588630A CN 201310624295 A CN201310624295 A CN 201310624295A CN 103588630 A CN103588630 A CN 103588630A
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Prior art keywords
copper stearate
type copper
hydrogen peroxide
environment
synthetic method
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CN201310624295.5A
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CN103588630B (en
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王从春
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SHANDONG GAOMI YOUHE AUXILIARY Co Ltd
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SHANDONG GAOMI YOUHE AUXILIARY Co Ltd
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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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)

Abstract

The present invention discloses an environmental-protection type copper stearate synthesis method, which comprises: adding stearic acid and basic copper carbonate to water according to a reaction molar ratio and a liquid-solid ratio of 8-12:1, uniformly stirring, adding a catalyst when heating to a temperature of 55-65 DEG C, continuously heating to a temperature of 75-85 DEG C, carrying out a reaction for 2-3 h to obtain blue copper stearate, and carrying out centrifugal dehydration to obtain the copper stearate product. According to the present invention, the environmental-protection type copper stearate synthesis method is provided, and has advantages of low reaction temperature, short reaction time and no byproduct generation during the reaction process, such that the production process is simple, the production efficiency is high, energy consumption and water consumption are low, the medium water and the waste heat can be used repeatedly, no environmental pollution problem exists, and the obtained product has advantages of high purity, less impurity and good color.

Description

A kind of synthetic method of environment-friendly type copper stearate
Technical field
The present invention relates to the preparation of stearate, be specifically related to a kind of synthetic method of environment-friendly type copper stearate.
Background technology
The catalyzer that copper stearate is produced as tensio-active agent, tertiary amine in rubber industry, the stain control agent in antifouling paint and being used widely.About the synthetic method of copper stearate, seldom, as the synthesis technique of stearates classics, be applied to industrial is mainly saponification one double decomposition and direct method to bibliographical information.The stearates that saponification one double decomposition is synthetic, comprises step saponification, metathesis, centrifuge dehydration, dry, has the low problem of production efficiency, and discharges a large amount of brine wastes, causes environmental protection pressure large.And the stearates of direct synthesis owing to must carrying out at higher temperature in building-up process, and needs reaction for a long time, so production energy consumption is high, production efficiency is low and oxidizing reaction easily occurs, and causes product color poor.And in the situation that not adding catalyzer more difficult the carrying out of reaction, if but added catalyzer, catalyzer is difficult to again remove, and causes product purity poor.
Summary of the invention
Technical problem to be solved by this invention is: the deficiency existing for prior art, provides that a kind of temperature of reaction is low, production efficiency is high, production cost is low, product purity is high, the synthetic method of the environment-friendly type copper stearate of non-environmental-pollution.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A synthetic method for environment-friendly type copper stearate, comprises the following steps:
By stearic acid with ventilation breather according to reacting mol ratio, according to the liquid-solid ratio of 8～12:1, be added to the water and stir, while being heated to 55～65 ℃, add catalyzer, continue to be warming up to 75～85 ℃, react and within 2～3 hours, obtain blue copper stearate, then through centrifuge dehydration, obtain copper stearate product.
As a kind of improvement, described catalyzer is hydrogen peroxide solution, and in described hydrogen peroxide solution, the add-on of hydrogen peroxide is 3～10% of stearic acid weight.
Preferably, the mass concentration of described hydrogen peroxide solution is 20～30%.
As further preferred, the mass concentration of described hydrogen peroxide solution is 27%, and the add-on of described hydrogen peroxide solution is 20～30% of stearic acid weight.
As a kind of preferably, described in add after catalyzer, continue to be warming up to 80 ℃, react and within 2～3 hours, obtain blue copper stearate.
Wherein, described stearic acid and ventilation breather by the mol ratio of reacting by following reaction formula, calculate:
4C 17H 35COOH+Cu(OH) 2·CuCO 3→2（C 17H 35COO） 2Cu+3H 2O+CO 2↑
As a kind of preferred, described liquid-solid ratio is 10:1.
Owing to having adopted technique scheme, the invention has the beneficial effects as follows:
The present invention is a kind of synthetic method of environment-friendly type copper stearate, that stearic acid and ventilation breather are under the katalysis of hydrogen peroxide, in water, synthesized copper stearate, its advantage is that temperature of reaction is low, the reaction times is short, reaction process no coupling product produces, therefore production technique is simple, production efficiency is high, energy consumption, water consumption are low, and WATER AS FLOW MEDIUM and waste heat can be recycled, and do not have problem of environmental pollution.And owing to adopting hydrogen peroxide as catalyzer, due to the unstable of hydrogen peroxide, in reaction process, decompose, therefore can not bring any impurity to product, so the product purity obtaining is high, impurity is few, color and luster good.Preparation method's of the present invention reaction conversion ratio reaches 1.03-1.05, in product, except containing a certain amount of moisture and free acid, there is no other impurity.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
By stearic acid with ventilation breather according to reacting mol ratio, according to the liquid-solid ratio of 8:1, be added to the water and stir, while being heated to 56 ℃, add catalyzer, continue to be warming up to 76 ℃, react and within 3 hours, obtain blue copper stearate, then through centrifuge dehydration, obtain copper stearate product, reaction conversion ratio is 1.03, moisture 0.59wt% in product, product purity 99.11wt%, free acid content 0.3wt%, copper content is 9.9wt%.
Embodiment 2
By stearic acid with ventilation breather according to reacting mol ratio, described stearic acid and ventilation breather by the mol ratio of reacting by following reaction formula, calculate: 4C 17h 35cOOH+Cu (OH) 2cuCO 3→ 2(C 17h 35cOO) 2cu+3H 2o+CO 2↑, according to the liquid-solid ratio of 9:1, be added to the water and stir, while being heated to 62 ℃, add hydrogen peroxide solution, in hydrogen peroxide solution, the weight of hydrogen peroxide is 10% of stearic acid weight, continues to be warming up to 82 ℃, reacts and within 2 hours, obtains blue copper stearate, then through centrifuge dehydration, obtain copper stearate product, reaction conversion ratio is 1.04, moisture 0.74wt% in product, product purity 99.01wt%, free acid content 0.25wt%, copper content is 10.1wt%.
Embodiment 3
By stearic acid with ventilation breather according to reacting mol ratio, according to the liquid-solid ratio of 11:1, be added to the water and stir, while being heated to 58 ℃, adding mass concentration is 25% hydrogen peroxide solution, in hydrogen peroxide solution, the weight of hydrogen peroxide is 8% of stearic acid weight, continue to be warming up to 78 ℃, react and within 2.5 hours, obtain blue copper stearate, then through centrifuge dehydration, obtain copper stearate product, reaction conversion ratio is 1.03, moisture 0.64wt% in product, product purity 99.15wt%, free acid content 0.21wt%, copper content is 10.35wt%.
Embodiment 4
By stearic acid with ventilation breather according to reacting mol ratio, described stearic acid and ventilation breather by the mol ratio of reacting by following reaction formula, calculate: 4C 17h 35cOOH+Cu (OH) 2cuCO 3→ 2(C 17h 35cOO) 2cu+3H 2o+CO 2↑, according to the liquid-solid ratio of 10:1, be added to the water and stir, while being heated to 60 ℃, adding mass concentration is 27% hydrogen peroxide solution, in hydrogen peroxide solution, the weight of hydrogen peroxide is 6% of stearic acid weight, continues to be warming up to 80 ℃, reacts and within 2 hours, obtains blue copper stearate, then through centrifuge dehydration, obtain copper stearate product, reaction conversion ratio is 1.05, moisture 0.60wt% in product, product purity 99.20wt%, free acid content 0.2wt%, copper content is 10.55wt%.

Claims (7)

1. a synthetic method for environment-friendly type copper stearate, is characterized in that comprising the following steps:
By stearic acid with ventilation breather according to reacting mol ratio, by the liquid-solid ratio of 8～12:1, be added to the water and stir, while being heated to 55～65 ℃, add catalyzer, continue to be warming up to 75～85 ℃, react and within 2～3 hours, obtain blue copper stearate, then through centrifuge dehydration, obtain copper stearate product.
2. the synthetic method of environment-friendly type copper stearate as claimed in claim 1, is characterized in that: described catalyzer is hydrogen peroxide solution, and in described hydrogen peroxide solution, the add-on of hydrogen peroxide is 3～10% of stearic acid weight.
3. the synthetic method of environment-friendly type copper stearate as claimed in claim 2, is characterized in that: the mass concentration of described hydrogen peroxide solution is 20～30%.
4. the synthetic method of environment-friendly type copper stearate as claimed in claim 3, is characterized in that: the mass concentration of described hydrogen peroxide solution is 27%, and the add-on of described hydrogen peroxide solution is 20～30% of stearic acid weight.
5. the synthetic method of environment-friendly type copper stearate as claimed in claim 1, is characterized in that: described in add after catalyzer, continue to be warming up to 80 ℃, react and within 2～3 hours, obtain blue copper stearate.
6. the synthetic method of the environment-friendly type copper stearate as described in claim as arbitrary in claim 1 to 5, is characterized in that: described stearic acid calculates by following reaction formula with the mol ratio of reacting of ventilation breather: 4C 17h 35cOOH+Cu (OH) 2cuCO 3→ 2(C 17h 35cOO) 2cu+3H 2o+CO 2↑.
7. the synthetic method of environment-friendly type copper stearate as claimed in claim 6, is characterized in that: described liquid-solid ratio is 10:1.
CN201310624295.5A 2013-11-28 2013-11-28 Environmental-protection type copper stearate synthesis method Active CN103588630B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113045403A (en) * 2021-03-08 2021-06-29 泰兴冶炼厂有限公司 Method for preparing copper stearate from acidic copper-containing etching waste liquid

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1837176A (en) * 2005-03-23 2006-09-27 广东工业大学 Process for preparation of metal stearate
CN101863759A (en) * 2010-06-12 2010-10-20 扬州工业职业技术学院 Method for preparing copper benzoate
CN102276441A (en) * 2011-04-20 2011-12-14 中山市华明泰化工材料科技有限公司 Environment-friendly metal carboxylate and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1837176A (en) * 2005-03-23 2006-09-27 广东工业大学 Process for preparation of metal stearate
CN101863759A (en) * 2010-06-12 2010-10-20 扬州工业职业技术学院 Method for preparing copper benzoate
CN102276441A (en) * 2011-04-20 2011-12-14 中山市华明泰化工材料科技有限公司 Environment-friendly metal carboxylate and preparation method thereof

Non-Patent Citations (2)

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Title
HUAIBIN SHEN ET AL: "Size-, shape-, and assembly-controlled synthesis of Cu2-xSe nanocrystals via a non-injection phosphine-free colloidal method", 《CRYSTENGCOMM.》, no. 14, 3 November 2011 (2011-11-03), pages 555 - 560 *
戴文娟: "硬脂酸锌的催化合成及其对PVC热解性能的影响研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, 15 April 2010 (2010-04-15) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113045403A (en) * 2021-03-08 2021-06-29 泰兴冶炼厂有限公司 Method for preparing copper stearate from acidic copper-containing etching waste liquid
CN113045403B (en) * 2021-03-08 2023-10-17 泰兴冶炼厂有限公司 Method for preparing copper stearate from acidic copper-containing etching waste liquid

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