CN105906473A - Preparation method of glyzinc - Google Patents
Preparation method of glyzinc Download PDFInfo
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- CN105906473A CN105906473A CN201610313336.2A CN201610313336A CN105906473A CN 105906473 A CN105906473 A CN 105906473A CN 201610313336 A CN201610313336 A CN 201610313336A CN 105906473 A CN105906473 A CN 105906473A
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- zinc
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- glycerol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/68—Preparation of metal alcoholates
- C07C29/70—Preparation of metal alcoholates by converting hydroxy groups to O-metal groups
Abstract
The invention relates to a preparation method of glyzinc, and belongs to the field of chemical synthesis. The preparation method comprises the following steps of adding a zinc source, a catalyst and an aprotic solvent into a reactor according to a mass ratio being 1:(0.05 to 0.15): (2 to 10); performing stirring for 5 to 30min; then, adding dispersing agents accounting for 0.3 to 3 percent of the mass of the zinc source; performing stirring for 5 to 10 min so that the zinc source and the catalyst are uniformly dispersed in a solvent; then, adding glycerol (the mol ratio of the glycerol to the zinc source is (1 to 1.2):1); raising the temperature to 100 to 150 DEG C under the stirring condition; taking a reaction for 2 to 4 hours; performing cooling and suction filtration; performing washing by C<1 to 3> monohydric alcohol, and then performing suction filtration and drying to obtain the glyzinc. The invention provides the preparation method with the advantages that the process is simple; the operation is convenient; the reaction conditions are mild; the temperature can be easily controlled. The glyzinc synthesis is performed in the aprotic solvents; through the addition of dispersing agents, reaction substances cannot agglomerate or deposit on the device wall; after the reaction, the filtering and the separation can be directly performed; the washing is easy.
Description
Technical field
The present invention relates to the preparation method of a kind of glycerin zinc, belong to the field of chemical synthesis.
Background technology
Glycerin zinc (Zinc glycerolate,
Glyzinc), glycerin zinc complex (Zinc glycerolate also it is
Complexes), molecular formula (C3H6O3Zn)x, it is a kind of broad-spectrum fine chemicals, there is good obstruct, uvioresistant performance, nontoxic, not colored, can be as the vulcanizing activator of the light stabilizer of plastics, heat stabilizer and rubber.Glycerin zinc is often used as the important component of cosmetics, plays the effects such as lubrication, anti-ultraviolet radiation, is also often used as zinc supplement agent and treats dermopathic medicine.At present, the preparation method of glycerin zinc is all to use zinc source and glycerol direct reaction, and glycerol consumption is usually 3-10 times of zinc source quality.Difference according to zinc source, reaction complexity and reaction condition are different: if employing zinc acetate is zinc source, then the reaction with glycerol is easier to carry out, without catalyst, glycerin zinc can be generated at 110 ~ 160 DEG C of direct reaction, but owing to zinc acetate cost is more expensive, and reaction produces intense stimulus and corrosive acetic acid, seldom uses in production；According to inorganic matter zinc sources such as zinc oxide, zinc carbonate, zinc hydroxide, it is generally required to the relatively harsh conditions such as catalysis, high temperature, pressurization, microwave reaction.Above-mentioned existing methodical common drawback is: be reactant and in the reaction system of solvent at glycerol, owing to viscosity is the biggest, initial stage stirring difficulty, after reaction terminates and cools down, glycerol forms paste-like thing with glycerin zinc, cause glycerin zinc to be difficult to split-phase with glycerol to separate, need centrifugal layering or mixture after the reaction pour the solvent dissolved each other with glycerol in a large number into, to facilitate filtration.Owing to there is the stronger effects such as hydrogen bond between glycerol and glycerin zinc, for removing absorption glycerol on glycerin zinc, it is necessary to repeatedly wash filter cake.Therefore, existing method is easily caused the loss of glycerol and cleaning solvent, causes environmental pollution.It addition, recovery glycerol and solvent will increase production cost.
Summary of the invention
The present invention is directed to the deficiency of existing glycerin zinc preparation method, it is provided that a kind of technique is simple and convenient to operate, reaction condition gentle, the preparation method of easy temperature control.Synthetic glycerine zinc of the present invention is to carry out in aprotic solvent, makes reactant be unlikely to conglomeration by interpolation dispersant and is deposited on wall, can directly filter separation after reaction, and easily washing obtains required product.
The glycerin zinc preparation method step of the present invention is as follows:
By zinc source: catalyst: the mass ratio of aprotic solvent is that 1:0.05 ~ 0.15:2 ~ 10 add in reactor, stirring 5 ~ 30min, is subsequently added into the dispersant of zinc source quality 0.3 ~ 3%, stirs 5 ~ 10min, make zinc source and catalyst dispersed in a solvent, being subsequently adding glycerol, glycerol is 1 ~ 1.2:1 with the mol ratio in zinc source, is under agitation warmed up to 100 ~ 150 DEG C, reaction 2 ~ 4h, cooling, sucking filtration, use C1~3Monohydric alcohol washing after, sucking filtration, be dried to obtain glycerin zinc of the present invention.
Described zinc source is zinc oxide, zinc carbonate or zinc hydroxide.
Described catalyst is C1~4Monocarboxylic acid compound and zinc salt, such as acetic acid, zinc formate, acrylic or methacrylic acid zinc.
Described aprotic solvent is boiling point 100 ~ 150 DEG C and the aprotic solvent immiscible with glycerol, such as hexahydrotoluene, toluene, n-propyl acetate or n-butyl acetate.
Described dispersant is glyceryl monostearate, Span-85, Span-80 or Span-60.
Described C1~3Monohydric alcohol is methanol, ethanol or isopropanol.
The present invention prepares the reaction temperature of glycerin zinc between 100 ~ 150 DEG C, specifically depending on the boiling point of the aprotic solvent used, and generally greater than solvent boiling point 1 ~ 2 DEG C.In this temperature range, the produced water of reaction can separate from system, it is ensured that reaction is quickly, completely.
Adhere to affect reaction on the reactor wall carry out owing to forming the pastel of thickness easily by hydrogen bonded between glycerol and zinc source, therefore, add after dispersant prevents zinc source absorption glycerol and be deposited on wall, it is ensured that zinc source and glycerol can disperse in a solvent.
The present invention compared with prior art, has the following characteristics that
1. using solvent to instead of the glycerol of excess, stirring is easier to, and the requirement to consersion unit is lower；
2. after reaction terminates cooling, it is formed without the paste-like thing of thickness, it is not necessary to centrifugation or separately add solvent to system, can directly filter, decrease processing step；
3. reaction temperature depends on the boiling point of used solvent, mild condition, is easily controlled；
4. the solvent collected after filtering, it is not necessary to distillation, can directly re-apply the preparation in glycerin zinc, does not discharge the garbage polluting environment.It it is a kind of easy and simple to handle, method preparing glycerin zinc of environmental protection.
Detailed description of the invention
Below by embodiment, technical scheme and effect are further elucidated with, but should not regard limiting the scope of the invention as.
Embodiment 1
30g zinc oxide, 1.5g zinc formate, 200g hexahydrotoluene is added in 1000mL is equipped with the there-necked flask of blender, thermometer, reflux condenser and water knockout drum, 0.6g glyceryl monostearate is added after stirring 5min, continue stirring 5min, it is subsequently added into 40.88g glycerol, under agitation it is warmed up to 110 DEG C, along with reaction is carried out, the water yield collected on water knockout drum is gradually increased, until after the reaction 3h water yield is not further added by, cooling, sucking filtration, wash 2 times with isopropanol, it is dried, obtains white powder glycerin zinc solid 57.20g.Being computed, the productivity of relative zinc oxide is 99.4%, and Zn content is 42.25%.
Embodiment 2
46g zinc carbonate, 4g acrylic acid, 180g n-propyl acetate is added in 500mL is equipped with the there-necked flask of blender, thermometer, reflux condenser and water knockout drum, 0.5g Span-60 is added after stirring 30min, continue stirring 10min, be subsequently added into 35g glycerol, be under agitation warmed up to 103 DEG C, reaction 4h, cooling, sucking filtration, wash 2 times with ethanol, it is dried, obtains white powder glycerin zinc solid 55.86g.Being computed, the productivity of relative zinc oxide is 96.65%, and Zn content is 42.81%.
Embodiment 3
30g zinc oxide, 3g acetic acid, 180g toluene is added in 500mL is equipped with the there-necked flask of blender, thermometer, reflux condenser and water knockout drum, 0.3g Span-80 is added after stirring 30min, continue stirring 5min, be subsequently added into 35.28g glycerol, be under agitation warmed up to 112 DEG C, reaction 2.5h, cooling, sucking filtration, wash 1 time with methanol, it is dried, obtains white powder glycerin zinc solid 56.66g.Being computed, the productivity of relative zinc oxide is 99.05%, and Zn content is 42.30%.
Embodiment 4
36.78g zinc hydroxide, 5g zinc methacrylate, 180g n-butyl acetate is added in 500mL is equipped with the there-necked flask of blender, thermometer, reflux condenser and water knockout drum, 0.3g Span-85 is added after stirring 5min, continue stirring 5min, be subsequently added into 35.50g glycerol, be under agitation warmed up to 128 DEG C, reaction 2h, cooling, sucking filtration, wash 1 time with isopropanol, it is dried, obtains white powder glycerin zinc solid 56.23g.Being computed, the productivity of relative zinc oxide is 98.30%, and Zn content is 42.53%.
Claims (8)
1. the preparation method of a glycerin zinc, it is characterised in that step is as follows:
By zinc source: catalyst: the mass ratio of aprotic solvent is that 1:0.05 ~ 0.15:2 ~ 10 add in reactor, stirring 5 ~ 30min, is subsequently added into the dispersant of zinc source quality 0.3 ~ 3%, stirs 5 ~ 10min, make zinc source and catalyst dispersed in a solvent, being subsequently adding glycerol, glycerol is 1 ~ 1.2:1 with the mol ratio in zinc source, is under agitation warmed up to 100 ~ 150 DEG C, reaction 2 ~ 4h, cooling, sucking filtration, use C1~3Monohydric alcohol washing after, sucking filtration, be dried to obtain glycerin zinc of the present invention.
The preparation method of glycerin zinc the most according to claim 1, it is characterised in that described zinc source is zinc oxide, zinc carbonate or zinc hydroxide.
The preparation method of glycerin zinc the most according to claim 1, it is characterised in that described catalyst is C1~4Monocarboxylic acid compound and zinc salt.
4. according to the preparation method of glycerin zinc described in claim 1 or 3, it is characterised in that described catalyst is acetic acid, zinc formate, acrylic or methacrylic acid zinc.
The preparation method of glycerin zinc the most according to claim 1, it is characterised in that described aprotic solvent is boiling point 100 ~ 150 DEG C and the aprotic solvent immiscible with glycerol.
6. according to the preparation method of glycerin zinc described in claim 1 or 5, it is characterised in that described aprotic solvent is hexahydrotoluene, toluene, n-propyl acetate or n-butyl acetate.
The preparation method of glycerin zinc the most according to claim 1, it is characterised in that described dispersant is glyceryl monostearate, Span-85, Span-80 or Span-60.
The preparation method of glycerin zinc the most according to claim 1, it is characterised in that described C1~3Monohydric alcohol is methanol, ethanol or isopropanol.
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| CN201610313336.2A CN105906473B (en) | 2016-05-12 | 2016-05-12 | A kind of preparation method of glycerin zinc |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320795A (en) * | 2018-09-25 | 2019-02-12 | 广东省稀有金属研究所 | A kind of organic zinc vulcanizing activator and preparation method thereof |
| CN109369478A (en) * | 2018-11-23 | 2019-02-22 | 广州天科生物科技有限公司 | A kind of synthetic method of zinc methionine chelate |
| KR20190140056A (en) * | 2017-05-03 | 2019-12-18 | 바스프 에스이 | Nucleating agents, methods for their preparation, and related polymer compositions |
| CN111533641A (en) * | 2020-05-16 | 2020-08-14 | 内蒙古联丰稀土化工研究院有限公司 | Preparation method of glycerin rare earth |
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| WO2004011409A1 (en) * | 2002-07-26 | 2004-02-05 | Micronisers Pty Ltd | Zinc glycerolate composition and method for manufacture thereof |
| CN101704721A (en) * | 2009-10-27 | 2010-05-12 | 中南民族大学 | Method for preparing glycerin zinc |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190140056A (en) * | 2017-05-03 | 2019-12-18 | 바스프 에스이 | Nucleating agents, methods for their preparation, and related polymer compositions |
| JP2020518677A (en) * | 2017-05-03 | 2020-06-25 | ビーエーエスエフ ソシエタス・ヨーロピアＢａｓｆ Ｓｅ | Nucleating agents, methods of making the same, and related polymer compositions |
| JP7184876B2 (en) | 2017-05-03 | 2022-12-06 | ビーエーエスエフ ソシエタス・ヨーロピア | Nucleating agents, methods of making same, and related polymer compositions |
| KR102550380B1 (en) | 2017-05-03 | 2023-07-04 | 바스프 에스이 | Nucleating agents, methods for their preparation, and related polymeric compositions |
| CN109320795A (en) * | 2018-09-25 | 2019-02-12 | 广东省稀有金属研究所 | A kind of organic zinc vulcanizing activator and preparation method thereof |
| CN109369478A (en) * | 2018-11-23 | 2019-02-22 | 广州天科生物科技有限公司 | A kind of synthetic method of zinc methionine chelate |
| CN111533641A (en) * | 2020-05-16 | 2020-08-14 | 内蒙古联丰稀土化工研究院有限公司 | Preparation method of glycerin rare earth |
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| CN105906473B (en) | 2018-12-28 |
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Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of rare metals, Guangdong Academy of Sciences Address before: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee before: GUANGDONG INSTITUTE OF RARE METALS |
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Effective date of registration: 20230406 Address after: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee after: Institute of resource utilization and rare earth development, Guangdong Academy of Sciences Address before: 510651 No. 363, Changxin Road, Guangzhou, Guangdong, Tianhe District Patentee before: Institute of rare metals, Guangdong Academy of Sciences |