CN102633617A - Method for preparing organic zinc by means of calcium analysis reactive crystallization - Google Patents
Method for preparing organic zinc by means of calcium analysis reactive crystallization Download PDFInfo
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- CN102633617A CN102633617A CN2012100865587A CN201210086558A CN102633617A CN 102633617 A CN102633617 A CN 102633617A CN 2012100865587 A CN2012100865587 A CN 2012100865587A CN 201210086558 A CN201210086558 A CN 201210086558A CN 102633617 A CN102633617 A CN 102633617A
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- terephthalic acid
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Abstract
The invention discloses a method for preparing organic zinc by means of calcium analysis reactive crystallization, which includes: adding terephthalic acid and water and/or filtrate in a reactor, and then adding sodium hydroxide to lead the terephthalic acid to dissolve into terephthalic acid sodium solution, wherein the filtrate is mother solution after centrifugal separation of organic zinc; adding saturated lime milk suspension to enable separation by crystallization of terephthalic acid calcium; adding saturated sodium zincate solution to enable separation by crystallization of terephthalic acid zinc on a terephthalic acid calcium carrier; and centrifuging, wherein filtrate which is sodium hydroxide solution is used for allocation of terephthalic acid sodium solution in next batch, so that an organic zinc product is obtained by rinsing and drying a centrifuged product. By the aid of the method, discharge of waste water containing inorganic salt such as sodium chloride and/or sodium sulfate and the like is avoided, the sodium hydroxide contained in centrifuged mother solution can be used for allocation of the terephthalic acid sodium solution in next batch, and consumption of the sodium hydroxide is reduced.
Description
[technical field]
The present invention relates to vulcanization of rubber acvator technical field, specifically, is that a kind of calcium that utilizes is analysed the method that reactive crystallization prepares organic zinc.
[background technology]
Rubber vulcanization system mainly comprises sulphur, promotor, acvator and Triple Pressed Stearic Acid; Wherein vulcanization activator is indispensable auxiliary agent; Vulcanization rate, cross-link bond type, cross-linking density and mechanical property etc. to sizing material produce material impact, and vulcanization activator commonly used is a zinc oxide.Yet; Zinc in the zinc oxide and heavy metal content are high, and the consumption in rubber and tire is very big, and zinc is discharged into the environment from rubber; For example discharge through Tyte Wear in the use; The release of zinc will cause environment is caused very big pollution, and health of human body is caused disadvantageous effect, especially the responsive aquatic animals and plants of zinc caused influence in various degree.On the other hand, zinc oxide density is big, is used for the rolling resistance that tire increases tire, is unfavorable for the target of tyre production enterprise realization green tire.
Organic zinc is a kind of vulcanization activator of low zinc content.Conventional organic zinc such as Zinic stearas, zinc laurate and zinc oleate etc. are brought into play various application in industries such as rubber, plastics jointly.
The conventional method for preparing organic zinc is known as fusion method, zn cpdss such as zinc oxide, oxidation zinc and/or zinc carbonate is heated in the presence of organic acids such as Triple Pressed Stearic Acid, oleic acid and/or other organic acid, to produce corresponding organic zinc.The organic zinc particle of this method preparation is thick, is difficult to pulverize, and result of use is undesirable.
The another kind of method for preparing organic zinc is with the reaction between one or more organic acid sodium salts, ammonium salt or sylvite and zinc sulfate, zinc acetate and/or the zinc chloride; Reaction product is precipitated out from aqueous reaction medium; Use water washing; To remove, dry then like by products such as sodium sulfate, sodium-chlor, ammonium sulfate.The organic zinc of this method preparation needs extra chemical reagent to carry out required conversion, produces the waste water of inorganic salt such as a large amount of contains sodium sulfate, sodium-chlor, ammonium sulfate in addition, and waste water can not directly discharge.
USP 2,492,314 utilize amine, dithiocarbonic anhydride and zinc oxide under anhydrous condition, to produce the organic zinc that comprises MGD, yet the product particle that obtains more slightly, bigger, use not ideal enough.USP 6,555,075 utilizes zinc-ammonia-carbonate complex compound and solution thereof to produce active zinc flower and/or zinc carbonate, consequent active zinc flower or zinc carbonate subsequently further with one or more organic acid reactions, make corresponding organic zinc salt.U.S. Patent application No. 2006/0281009, No. 2008/0194748 and No. 2008/0161475 communique, and USP 6,291; 572 and 6; 333,375th, utilize the method for coating, organic salt is coated contained silicon grain; Like precipitated silica, clay, kaolin, talcum, pure aluminium silicate, lime carbonate, carbon black and composition thereof; Said coated particle has been given favourable characteristic to the rubber item that is formed by it when adding to rubber combination as filler, comprise improving wear resistance, modulus and tensile strength.Chinese invention patent application 200980152769.2 is adopted and is generated zinc ammonia complex; Use one or more organic acids and/or its salt to handle described complex compound subsequently; Thereby formation organic zinc, said method have been avoided such sodium-chlor and/or sodium sulfate byproduct of forming in the ordinary method.
[summary of the invention]
The purpose of this invention is to provide a kind of calcium and analyse the method that reactive crystallization prepares organic zinc, non-sodium chloride and/or sodium sulfate etc. contain the inorganic salt discharge of wastewater in the production process, produce the centrifuge mother liquor recycle of organic zinc.
Implementation method of the present invention is:
In reaction kettle, add terephthalic acid, add water and/or filtrating; Wherein filtrating is the mother liquor behind the spinning organic zinc, and adding sodium hydroxide makes terephthalic acid be dissolved as the terephthalic acid sodium solution, adds saturated lime cream soliquoid; Make its crystallization separate out terephthalic acid calcium, add saturated sodium zincate solution, make it on terephthalic acid calcium, continue crystallization and separate out terephthalic acid zinc; Centrifugal afterwards, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.Centrifugal product is the organic zinc product through washing, oven dry.
The present invention realizes that through following technical scheme its concrete steps are:
(1) in reaction kettle, add 20～100 parts of terephthalic acids, add water and/or filtrate 80～300 parts, add 5～100 parts in sodium hydroxide, stir;
(2) treat terephthalic acid dissolving fully after, add 5～100 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit stirs, 30～120 rev/mins of stir speed (S.S.)s added in 10～60 minutes;
(3) add 5～100 parts of saturated sodium zincate solution, the limit edged stirs, and 30～120 rev/mins of stir speed (S.S.)s added in 10～60 minutes.
(4) standing sedimentation is 30～120 minutes;
(5) spinning, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.
The centrifugal product that obtains through washing, oven dry, is the organic zinc product.
Compared with prior art; Positively effect of the present invention is: the present invention utilizes calcium to analyse the organic zinc of reaction crystallizing method preparation; Non-sodium chloride and/or sodium sulfate etc. contain the inorganic salt discharge of wastewater; And contained sodium hydroxide can be used for the configuration of next batch terephthalic acid sodium solution in the centrifuge mother liquor, has saved the consumption of sodium hydroxide.
[description of drawings]
Fig. 1 calcium is analysed reactive crystallization and is prepared organic zinc technological line figure.
[embodiment]
Below provide calcium of the present invention to analyse the embodiment that reactive crystallization prepares organic zinc.
Embodiment 1
In reaction kettle, add 80 parts of terephthalic acids, add 160 parts in water, add 60 parts in sodium hydroxide, stir.After treating terephthalic acid dissolving fully, add 60 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit stirs, and 60 rev/mins of stir speed (S.S.)s added in 20 minutes.Standing sedimentation 60 minutes adds 60 parts of saturated sodium zincate solution, and the limit edged stirs, and 30 rev/mins of stir speed (S.S.)s added in 60 minutes.Standing sedimentation 60 minutes.Spinning, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.The centrifugal product that obtains through washing, oven dry, is the organic zinc product.
Embodiment 2
In reaction kettle, add 80 parts of terephthalic acids, add 120 parts of filtratings, add 10 parts in sodium hydroxide, stir.After treating terephthalic acid dissolving fully, add 60 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit stirs, and 60 rev/mins of stir speed (S.S.)s added in 20 minutes.Standing sedimentation 60 minutes adds 60 parts of saturated sodium zincate solution, and the limit edged stirs, and 60 rev/mins of stir speed (S.S.)s added in 30 minutes.Standing sedimentation 30 minutes.Spinning, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.The centrifugal product that obtains through washing, oven dry, is the organic zinc product.
Embodiment 3
In reaction kettle, add 80 parts of terephthalic acids, add 120 parts of filtratings, add 80 parts in sodium hydroxide, stir.After treating terephthalic acid dissolving fully, add 80 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit stirs, and 60 rev/mins of stir speed (S.S.)s added in 60 minutes.Standing sedimentation 60 minutes adds 80 parts of saturated sodium zincate solution, and the limit edged stirs, and 60 rev/mins of stir speed (S.S.)s added in 60 minutes.Standing sedimentation 60 minutes.Spinning, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.The centrifugal product that obtains through washing, oven dry, is the organic zinc product.
Embodiment 4
In reaction kettle, add 60 parts of terephthalic acids, add 80 parts of filtratings, add 20 parts in sodium hydroxide, stir.After treating terephthalic acid dissolving fully, add 10 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit stirs, and 60 rev/mins of stir speed (S.S.)s added in 20 minutes.Standing sedimentation 40 minutes adds 20 parts of saturated sodium zincate solution, and the limit edged stirs, and 60 rev/mins of stir speed (S.S.)s added in 30 minutes.Standing sedimentation 120 minutes.Spinning, filtrating is sodium hydroxide solution, is used to dispose next batch terephthalic acid sodium solution.The centrifugal product that obtains through washing, oven dry, is the organic zinc product.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some improvement and retouching, these improvement and retouching also should be regarded as in protection scope of the present invention.
Claims (5)
1. a calcium is analysed the method that the nuclear reaction crystallization of contracting prepares organic zinc, it is characterized in that concrete steps are:
In reaction kettle, add terephthalic acid, add water and/or filtrating; Wherein filtrating is the mother liquor behind the spinning organic zinc, and adding sodium hydroxide makes terephthalic acid be dissolved as the terephthalic acid sodium solution, adds saturated lime cream soliquoid; Make its crystallization separate out terephthalic acid calcium, add saturated sodium zincate solution, make its crystallization on terephthalic acid calcium carrier separate out terephthalic acid zinc; Centrifugal afterwards, filtrating is sodium hydroxide solution, is used to dispose next batch terephthaldehyde acid solution.The centrifugal organic zinc that obtains is product through washing, oven dry.
2. analyse the method that the nuclear reaction crystallization of contracting prepares organic zinc like claims 1 described a kind of calcium, it is characterized in that, 20～100 parts of the terephthalic acids of adding, the water of adding and/or filtrate 80～300 parts, 5～100 parts in the sodium hydroxide of adding.
3. analyse the method that the nuclear reaction crystallization of contracting prepares organic zinc like claims 1 described a kind of calcium; It is characterized in that, add 5～100 parts of saturated lime cream soliquoids, the limit adds saturated lime cream soliquoid limit and stirs; 30～120 rev/mins of stir speed (S.S.)s added in 10～60 minutes.
4. analyse the method that the nuclear reaction crystallization of contracting prepares organic zinc like claims 1 described a kind of calcium, it is characterized in that, add 5～100 parts of saturated sodium zincate solution; The limit edged stirs; Stir speed (S.S.) is 30～120 rev/mins, adds in 10～60 minutes, and time of repose is 30～120 minutes afterwards.
5. analysing the method that the nuclear reaction crystallization of contracting prepares organic zinc like claims 1 described a kind of calcium, it is characterized in that, is diluted sodium hydroxide solution in the filtrating after the spinning, is used to dispose next batch terephthalic acid sodium solution, to save the sodium hydroxide consumption.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103554783A (en) * | 2013-11-04 | 2014-02-05 | 江苏爱特恩东台新材料科技有限公司 | Method for preparing PVC (polyvinyl vinyl chloride) calcium-zinc complex heat stabilizer through crude terephthalic acid |
| CN103833547A (en) * | 2014-01-27 | 2014-06-04 | 江苏爱特恩东台新材料科技有限公司 | Method and device for producing organic zinc by utilization of ultrasonic tubular reactor |
| CN104119220A (en) * | 2013-04-23 | 2014-10-29 | 陈祥迎 | Aluminium terephthalate PVC heat stabilizer and preparation method thereof |
| CN110256233A (en) * | 2019-06-28 | 2019-09-20 | 常州大学 | A kind of preparation method of organic metal carboxylate |
| WO2020258441A1 (en) * | 2019-06-28 | 2020-12-30 | 常州大学 | Preparation method for nano organometallic carboxylate |
-
2012
- 2012-03-28 CN CN2012100865587A patent/CN102633617A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104119220A (en) * | 2013-04-23 | 2014-10-29 | 陈祥迎 | Aluminium terephthalate PVC heat stabilizer and preparation method thereof |
| CN103554783A (en) * | 2013-11-04 | 2014-02-05 | 江苏爱特恩东台新材料科技有限公司 | Method for preparing PVC (polyvinyl vinyl chloride) calcium-zinc complex heat stabilizer through crude terephthalic acid |
| CN103554783B (en) * | 2013-11-04 | 2017-02-08 | 江苏爱特恩东台新材料科技有限公司 | Method for preparing PVC (polyvinyl vinyl chloride) calcium-zinc complex heat stabilizer through crude terephthalic acid |
| CN103833547A (en) * | 2014-01-27 | 2014-06-04 | 江苏爱特恩东台新材料科技有限公司 | Method and device for producing organic zinc by utilization of ultrasonic tubular reactor |
| CN110256233A (en) * | 2019-06-28 | 2019-09-20 | 常州大学 | A kind of preparation method of organic metal carboxylate |
| WO2020258442A1 (en) * | 2019-06-28 | 2020-12-30 | 常州大学 | Preparation method for organic metal carboxylate |
| WO2020258441A1 (en) * | 2019-06-28 | 2020-12-30 | 常州大学 | Preparation method for nano organometallic carboxylate |
| US11555043B2 (en) | 2019-06-28 | 2023-01-17 | Changzhou University | Preparation method for nano organometallic carboxylate |
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Application publication date: 20120815 |