CN104387257A - Method for preparing lithium stearate - Google Patents
Method for preparing lithium stearate Download PDFInfo
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- CN104387257A CN104387257A CN201410756626.5A CN201410756626A CN104387257A CN 104387257 A CN104387257 A CN 104387257A CN 201410756626 A CN201410756626 A CN 201410756626A CN 104387257 A CN104387257 A CN 104387257A
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- lithium
- lithium stearate
- stearic acid
- stearate
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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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for preparing lithium stearate. The method comprises the following steps: feeding stearic acid to a reaction kettle at ordinary pressure, and heating to 145-205 DEG C; adding lithium hydroxide and a catalyst in two steps, enabling the stearic acid to react with lithium hydroxide under the action of the catalyst; adding an antioxidant, stirring, and spraying the molten lithium stearate through a spray head in a mist form; cooling cold air flowing upwards below the spray head into a microparticle shape; and collecting and drying to obtain the lithium stearate. The catalyst adopted by the method is a lithium salt compound; the raw material lithium hydroxide reacts to generate the lithium stearate; the catalyst can further react with the lithium stearate; impurities are reduced; and therefore, the method has great popularization and application value.
Description
Technical field
The present invention relates to promoter material preparation field, be specifically related to the preparation method of lithium stearate.
Background technology
In plastics extrusion moulding process, required inside and outside lubricant agent object is to improve its processing performance, not occurring or occur less that melt is attached on metallic surface phenomenon, ensures the visual appearance of goods, and the auxiliary agent added in formula; In melt moulding process, play lubrication, make the easy demoulding of goods or the auxiliary agent from roller, be called lubricant.
The performance requriements of lubricant is: 1, must have excellent, imitate endurable lubricity.2, possess good consistency with polymkeric substance, inner, external lubrication effect will balance, and does not affect the transparency of resin, non-blooming, less scaling, does not react with other auxiliary agents.3, surface traction is little, and viscosity is little, in the favorable expandability of interface, easily forms interface consistency.4, thermal stability is excellent, does not decompose, non-volatile in machine-shaping process.5, do not reduce the various premium propertiess of polymkeric substance as far as possible, do not affect the suitability for secondary processing of plastics; 6, nontoxic, pollution-free, not etching apparatus, low price.
Though lubricant can not improve inner quality and the performance of plastics, be also absolutely necessary additive in plastic working.Its performance and effect have a certain impact to the quality tool after the workability of plastics and processing.Therefore, the character of lubricant, effect and application regularity is grasped very necessary and important.
Lithium stearate, another name stearic acid lithium salts, lithium stearate is mainly used for the auxiliary formula of plastic material in the plastic, has thermally-stabilised and lubricant effect, and compared with other stearate, its fusing point is higher, has better thermostability.Described lithium stearate is compared with Zinic stearas of the same type, calcium stearate, and it is subject to pursuing energetically of plastic cement processing enterprise.
Preparation method at present about lithium stearate discloses less, and I takes charge of a large amount of manpower and materials of input and research and develop, and has carried out a series of exploration and improvement to the preparation method of lithium stearate.
Summary of the invention
Object of the present invention provides a kind of preparation method of lithium stearate, can make the output of raising lithium stearate, and the lithium stearate produced is directly particulate state, and foreign matter content is few, and quality is high.
For realizing object of the present invention, the invention provides following technical scheme:
The preparation method of lithium stearate, comprises step as follows: put in reactor by stearic acid at ambient pressure and be heated to 145-205 DEG C; Add lithium hydroxide, catalyzer in two steps, stearic acid and lithium hydroxide react under the effect of catalyzer; Add oxidation inhibitor to stir; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Described catalyzer is: one or more in Lithium oxychloride, lithium peroxide, lithium nitrite, lithium nitrite, propyl alcohol, Virahol and hydrogen phosphite lithium.
Described oxidation inhibitor is: one or more of formaldehyde, distearyl pentaerythritol diphosphite (618), tris phosphite (168), acetaldehyde, lithium bromate.
The ratio of weight and number of described stearic acid and lithium hydroxide, catalyzer, oxidation inhibitor is: stearic acid 80-92; Lithium hydroxide 6-10; Catalyzer 1-5; Oxidation inhibitor 1-3.
Described stearic acid and lithium hydroxide react 50-100 minute under the effect of promotor, and after adding oxidation inhibitor, churning time is 8-15 minute.
The speed of described shower nozzle ejection lithium stearate can regulate, and the speed that the granular size of lithium stearate and shower nozzle spray is inverse ratio.
The cold wind humidity upwards flowed below described shower nozzle is more than 60%, dissolves and take away with cold wind in the cold wind of the impurities dissolves in lithium stearate particle more than 60% humidity.
The invention has the advantages that:
1, the catalyzer that the present invention adopts is lithium salt compound, and after making feed hydrogen Lithium Oxide 98min react generation lithium stearate, catalyzer can continue reaction with stearic acid, decreases the generation of impurity.
2, directly lithium stearate made particulate state in job shop and collect, effectively improving the environmental quality in workshop, greatly reduce the healthy effect to shop worker.
3, in the cold wind that adopts of the present invention, humidity is comparatively large, and impurity can be taken out of with cold wind, while cooling, carried out a dedoping step, simple to operate, feasibility is strong.
Embodiment
In order to illustrate in greater detail the present invention, providing and followingly preparing example.But scope of the present invention is not limited thereto.
Embodiment 1:
Get stearic acid 910g to drop in reactor, be heated to 140 DEG C, drop into 60g lithium hydroxide and catalyzer lithium nitrite 20g, react and add oxidation inhibitor formaldehyde 10g after 60 minutes, stir 10 minutes; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Embodiment 2
Get stearic acid 900g to drop in reactor, be heated to 145 DEG C, drop into 70g lithium hydroxide and catalyzer lithium nitrite 15g, react and add oxidation inhibitor distearyl pentaerythritol diphosphite (618) 15g after 100 minutes, stir 8 minutes; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Embodiment 3
Get stearic acid 920g to drop in reactor, be heated to 145 DEG C, drop into 65g lithium hydroxide and catalyzer lithium nitrite 15g, react and add oxidation inhibitor tris phosphite (168) 10g after 80 minutes, stir 12 minutes; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Embodiment 4:
Getting stearic acid 920g drops in reactor, be heated to 145 DEG C, drop into 65g lithium hydroxide and catalyzer lithium nitrite 15g, react after 80 minutes, the lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Embodiment 5:
Get stearic acid 920g to drop in reactor, be heated to 145 DEG C, drop into 65g lithium hydroxide, react and add oxidation inhibitor formaldehyde 10g after 80 minutes, stir 12 minutes; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
Embodiment 6:
Get stearic acid 920g to drop in reactor, be heated to 145 DEG C, drop into 65g lithium hydroxide, react 80 minutes; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
The lithium stearate that above embodiment is obtained carries out performance test, and whiteness data are that whiteness instrument detects; High temperature resistant experimental data obtains in constant temperature oven, and experiment condition is: constant temperature 220 DEG C, constant temperature time 120 minutes.
The following form of test result:
| Parameter | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Acid number | 0.1 | 0.1 | 0.1 | 0.2 | 0.3 | 0.4 |
| Whiteness (before constant temperature) | 97 | 96 | 97 | 95 | 94 | 95 |
| Whiteness (after constant temperature) | 90 | 91 | 92 | 78 | 80 | 50 |
Can be drawn by list data, the aspect of performance of preparation method of the present invention after constant temperature, have obvious advantage, and acid number is lower, improves processing characteristics.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, any those of ordinary skill in the art are in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (7)
1. the preparation method of lithium stearate, comprises step as follows: put in reactor by stearic acid at ambient pressure and be heated to 145-205 DEG C; Add lithium hydroxide, catalyzer in two steps, stearic acid and lithium hydroxide react under the effect of catalyzer; Add oxidation inhibitor to stir; The lithium stearate of melting is sprayed by shower nozzle vaporific, under the cooling of the cold wind upwards flowed below shower nozzle, is cooled to microparticle shape; Collect to dry and obtain described lithium stearate.
2. the preparation method of lithium stearate according to claim 1, described catalyzer is: one or more in Lithium oxychloride, lithium peroxide, lithium nitrite, lithium nitrite, propyl alcohol, Virahol and hydrogen phosphite lithium.
3. the preparation method of lithium stearate according to claim 1, described oxidation inhibitor is: one or more of formaldehyde, distearyl pentaerythritol diphosphite (618), tris phosphite (168), acetaldehyde, lithium bromate.
4. the preparation method of lithium stearate according to claim 1, the ratio of weight and number of described stearic acid and lithium hydroxide, catalyzer, oxidation inhibitor is: stearic acid 80-92; Lithium hydroxide 6-10; Catalyzer 1-5; Oxidation inhibitor 1-3.
5. the preparation method of lithium stearate according to claim 1, described stearic acid and lithium hydroxide react 50-100 minute under the effect of promotor, and after adding oxidation inhibitor, churning time is 8-15 minute.
6. the preparation method of lithium stearate according to claim 1, the speed of described shower nozzle ejection lithium stearate can regulate, and the speed that the granular size of lithium stearate and shower nozzle spray is inverse ratio.
7. the preparation method of lithium stearate according to claim 1, the cold wind humidity upwards flowed below described shower nozzle is more than 60%, dissolves and take away with cold wind in the cold wind of the impurities dissolves in lithium stearate particle more than 60% humidity.
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| CN201410756626.5A CN104387257B (en) | 2014-12-11 | 2014-12-11 | The preparation method of lithium stearate |
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| CN201410756626.5A CN104387257B (en) | 2014-12-11 | 2014-12-11 | The preparation method of lithium stearate |
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| CN104387257A true CN104387257A (en) | 2015-03-04 |
| CN104387257B CN104387257B (en) | 2017-03-15 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205179A (en) * | 2019-06-11 | 2019-09-06 | 中山华明泰科技股份有限公司 | A kind of preparation method and application of hydroxy fatty acid lithium |
Citations (6)
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| JPS5798235A (en) * | 1980-12-10 | 1982-06-18 | Nippon Oil & Fats Co Ltd | Preparation of metallic soap |
| US6339049B1 (en) * | 1999-11-10 | 2002-01-15 | Thk Co., Ltd. | Grease compositions and bearings sealed therewith |
| CN101045681A (en) * | 2007-04-30 | 2007-10-03 | 豫越(宁波)化工科技有限公司 | Method for producing heavy stearate by reaction extrusion process of screus reactor |
| CN101914007A (en) * | 2010-08-06 | 2010-12-15 | 东莞市汉维新材料科技有限公司 | Method for preparing high-temperature resistant zinc stearate |
| CN103044232A (en) * | 2012-12-17 | 2013-04-17 | 浙江赞宇科技股份有限公司 | Process for preparing stearate by low temperature ball-milling method |
| CN103044233A (en) * | 2012-12-17 | 2013-04-17 | 杭州油脂化工有限公司 | Process for preparing stearate through ball milling |
-
2014
- 2014-12-11 CN CN201410756626.5A patent/CN104387257B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5798235A (en) * | 1980-12-10 | 1982-06-18 | Nippon Oil & Fats Co Ltd | Preparation of metallic soap |
| US6339049B1 (en) * | 1999-11-10 | 2002-01-15 | Thk Co., Ltd. | Grease compositions and bearings sealed therewith |
| CN101045681A (en) * | 2007-04-30 | 2007-10-03 | 豫越(宁波)化工科技有限公司 | Method for producing heavy stearate by reaction extrusion process of screus reactor |
| CN101914007A (en) * | 2010-08-06 | 2010-12-15 | 东莞市汉维新材料科技有限公司 | Method for preparing high-temperature resistant zinc stearate |
| CN103044232A (en) * | 2012-12-17 | 2013-04-17 | 浙江赞宇科技股份有限公司 | Process for preparing stearate by low temperature ball-milling method |
| CN103044233A (en) * | 2012-12-17 | 2013-04-17 | 杭州油脂化工有限公司 | Process for preparing stearate through ball milling |
Non-Patent Citations (1)
| Title |
|---|
| 周家春主编: "《食品工业新技术》", 31 January 2005, article "喷雾冷却法", pages: 234-236 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110205179A (en) * | 2019-06-11 | 2019-09-06 | 中山华明泰科技股份有限公司 | A kind of preparation method and application of hydroxy fatty acid lithium |
| CN110205179B (en) * | 2019-06-11 | 2021-08-17 | 中山华明泰科技股份有限公司 | Preparation method and application of hydroxy fatty acid lithium |
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| CN104387257B (en) | 2017-03-15 |
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Address after: 523000 Luqiao Bridge Town, Dongguan, a new bridge west street, Tai Po, No. 5 Applicant after: DONGGUAN CHNV TECHNOLOGY CO., LTD. Address before: 523000 Luqiao Bridge Town, Dongguan, a new bridge west street, Tai Po, No. 5 Applicant before: CHNV Material Technology Co., Ltd. |
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