CN1326590C - Preparation method of industrial defoaming agent - Google Patents
Preparation method of industrial defoaming agent Download PDFInfo
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- CN1326590C CN1326590C CNB2005100345830A CN200510034583A CN1326590C CN 1326590 C CN1326590 C CN 1326590C CN B2005100345830 A CNB2005100345830 A CN B2005100345830A CN 200510034583 A CN200510034583 A CN 200510034583A CN 1326590 C CN1326590 C CN 1326590C
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- glycerine
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- defoaming agent
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Abstract
The present invention relates to a preparation method of industrial defoaming agents, which belongs to the manufacture field of organic chemical industry defoaming agents. The method comprises the following steps: first, under the condition of a catalyst, polymerizing glycerine into polyglycerine with the polymerization degree at 2 to 10, then adding in glycerine fatty acid ester or fatty acid according to the determined mass ratio for ester exchange, and obtaining products of the present invention. The present invention has the advantages of simple and convenient production processes, easy availability of materials, good defoaming and foam-suppressing effect and suitability for processes, such as paper making, sugar manufacturing, ferment, etc.
Description
Technical field
The present invention relates to a kind of preparation method of industrial defoaming agent, prepared defoamer is applicable to froth breaking in papermaking, printing and dyeing, fermentation, the sugar refining technology, presses down bubble.
Background technology
In papermaking, printing and dyeing, fermentation and sugar refining technology process, often have a large amount of foams and produce, influence carrying out smoothly of technical process,, must use the defoamer elimination or reduce foam in order to guarantee to produce.
At present defoamer is of a great variety, mainly contains the grease class, polyethers, polysiloxane-based and sulfonation grease etc.But the application of these defoamers all has certain limitation, and has complex manufacturing, costs an arm and a leg or use shortcomings such as inconvenience, and is particularly not good in industrial results of use such as papermaking, sugarings.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of defoamer, prepared defoamer is applied in papermaking, printing and dyeing, fermentation and the sugar refining technology good froth breaking and suds suppressing properties are arranged, and produces easily, and is easy to use.
Purpose of the present invention is achieved through the following technical solutions:
First step polymerization
With glycerine is raw material, stirs to heat up and the adding catalyst, and 180 °-250 ℃ reactions 1-5 hour, getting the degree of polymerization was the polymerization glycerine of 2-10, and its reaction equation is as follows:
n=2~10
The second step ester exchange
Get above-mentioned polymerization glycerine 15-65 mass parts, about 120 ℃ of preheatings add fatty acid glyceride or aliphatic acid 35-85 mass parts, and little amount of catalyst, 150 ℃-250 ℃ stirring reaction 2-4 hour.
Reaction equation:
n=2~10 m=8~18 x=1~3
Best catalyst is KOH or NaOH in the two-step reaction, Na
2CO
3, K
2CO
3, MnO
2, can be one or more.
Be product of the present invention through the reacted waxy solid of above-mentioned ester exchange (or esterification).
Product of the present invention has good defoaming effect, as will further improving antifoam performance, product 60-65 mass parts after the also desirable above-mentioned second step ester exchange, add dimethicone 2-5 mass parts, white carbon black 1-3 mass parts, sorbester p17 and Tween 80 2-5 mass parts, water 30-35 mass parts, disperseed 5-15 minute under rotating speed 800~1000rpm with dispersion machine, get yellow-white paste object.This product has good froth breaking, suds suppressing properties.
In order to check the defoaming effect of product, the present invention uses a kind of special apparatus and method, and is specific as follows:
(1) instrument and equipment: one in 500ml graduated cylinder, one of the air pump of flow 1~2L/min (disperser of band gas).
(2) reagent:
The sample configuration: sample disperses dilution with distilled water, and the ratio of sample and water is 1: 30
Expanding foam solution: expanding foam solution uses the process fluid that produces foam in the practical application, when being used to refine sugar process, with the syrup of 50 ° of BX, is heated to 70 ℃.
(3) method of operating
Measure the 100ml expanding foam solution in the 500ml graduated cylinder, the unlatching air pump makes and bubbles to 500ml, adds 1ml rapidly and has diluted good defoamer, calculates the time when foam drops to liquid level thus, is foam time.Again open air pump, the time when foam rises to 300ml again is for pressing down the bubble time.When sugar industry was used, foam time should be less than 30 seconds, and pressing down the bubble time should be greater than 5 minute.
The specific embodiment
Embodiment 1
Get the 250ml there-necked flask, load onto stirring, heater, and division box, take by weighing glycerine 138g (1.5mol) and add in the there-necked flask, stir and be warming up to 100 ℃, add catalyst 1.5g, be warming up to 230 ℃, reacted two hours, must the little yellow polyglycereol product of about 115g.
Embodiment 2
Reaction unit is an example 1, takes by weighing glycerine 184g (2mol), stirs and is warming up to about 100 ℃, adds catalyst 4g, continues to be warming up to 230 ℃, reacts four hours, gets the about 150g of little yellow polyglycereol product.
Embodiment 3
Get the 250ml there-necked flask, load onto stirring, heater, get the polyglycereol product 120g of example 1 gained, be warming up to 120 ℃, add stearic acid 80g (0.25mol) and catalyst 2g, being warming up to 200 ℃ stirred three hours, must about 160g product, outward appearance is the brownish black waxy solid, emulsification in hot water, foam time 28 seconds presses down the bubble time greater than 5 minutes (expanding foam solution syrup).
Embodiment 4
Reaction unit such as example 3 are got example 1 or example 2 polyglycereol 30g, oleic acid 150g, catalyst 6g, 200 ℃ of down reactions three hours, must with the about 180g of example 3 similar products, foam time 38 seconds, but the bubble time was greater than 10 minutes (expanding foam solution was a syrup).
Embodiment 5
Reaction unit such as example 3 are got example 1 or example 2 polyglycereol 80g, lard 80g, and catalyst 10g, 200 ℃ were reacted three hours, got the about 160g of example 3 similar products, and foam time is 25 seconds, presses down the bubble time greater than 5 minutes (expanding foam solution is a syrup).
Embodiment 6
Reaction unit such as example 3 are got example 1 or example 2 polyglycereol 80g, vegetable oil 60g, and catalyst 10g, 200 ℃ were reacted three hours, got the about 150g of example 3 similar products, and foam time is 35 seconds, presses down the bubble time greater than 8 minutes (expanding foam solution is a syrup).
Embodiment 7
Get example 3 or example 4, example 5, example 6 product 100g, add dimethicone 5g, white carbon black 1g, water 50g, and sorbester p17 and Tween 80 4g are 800 to 1000rpm under to disperse 10 minute with dispersion machine at rotating speed with the laboratory, get yellow-white paste object, this product has good froth breaking and suds suppressing properties.
Claims (3)
1, a kind of preparation method of industrial defoaming agent is characterized in that comprising the steps:
(1) with glycerine be raw material, stir and heat up and the adding catalyst that 180 ℃-250 ℃ reactions 1-5 hour, getting the degree of polymerization was the polymerization glycerine of 2-10, wherein said catalyst is KOH, NaOH, Na
2CO
3, K
2CO
3, MnO
2In one or more;
(2) get above-mentioned polymerization glycerine 15-65 mass parts, add fatty acid glyceride or aliphatic acid 35-85 mass parts after the preheating, and identical catalyst in adding and the step (1), 150 ℃-250 ℃ stirring reaction 2-4 hour.
2, the preparation method of industrial defoaming agent according to claim 1 is characterized in that described fatty acid glyceride or aliphatic acid are stearic acid or vegetable oil or oleic acid or lard.
3, a kind of preparation method of industrial defoaming agent, it is characterized in that the product 60-65 mass parts that makes with claim 1 step (2), add dimethicone 2-5 mass parts, white carbon black 1-3 mass parts, sorbester p17 and Tween 80 2-5 mass parts, water 30-35 mass parts is to disperse 5-15 minute under the 800-1000rpm with dispersion machine at rotating speed.
Priority Applications (1)
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CNB2005100345830A CN1326590C (en) | 2005-05-16 | 2005-05-16 | Preparation method of industrial defoaming agent |
Applications Claiming Priority (1)
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CNB2005100345830A CN1326590C (en) | 2005-05-16 | 2005-05-16 | Preparation method of industrial defoaming agent |
Publications (2)
Publication Number | Publication Date |
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CN1721031A CN1721031A (en) | 2006-01-18 |
CN1326590C true CN1326590C (en) | 2007-07-18 |
Family
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CNB2005100345830A Expired - Fee Related CN1326590C (en) | 2005-05-16 | 2005-05-16 | Preparation method of industrial defoaming agent |
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Families Citing this family (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101791495B (en) * | 2010-03-19 | 2011-12-28 | 新时代(济南)民爆科技产业有限公司 | Defoamer suitable for amino acid fermentation production |
WO2012127961A1 (en) * | 2011-03-23 | 2012-09-27 | 理研ビタミン株式会社 | Defoaming agent for food |
CN102382861B (en) * | 2011-07-25 | 2014-03-12 | 广州甘蔗糖业研究所 | Defoaming agent used for molasses alcohol fermentation |
CN102580361B (en) * | 2012-02-21 | 2014-07-30 | 广州甘蔗糖业研究所 | Defoaming agent for sugar industry and preparation method for defoaming agent |
CN102669506B (en) * | 2012-05-10 | 2014-01-29 | 河南正通化工有限公司 | Refining method for polyglycerin and polyglycerin fatty acid ester |
CN103387883A (en) * | 2012-05-11 | 2013-11-13 | 天津博克尼科技发展有限公司 | Method for preparing sorbitan fatty acid ester by utilizing waste oil through ester exchange process |
CN103818979A (en) * | 2012-11-16 | 2014-05-28 | 季爱英 | Defoaming agent for papermaking |
CN103818980A (en) * | 2012-11-16 | 2014-05-28 | 季爱英 | Defoaming agent for printing and dyeing wastewater |
CN106267910A (en) * | 2016-08-10 | 2017-01-04 | 中国海洋石油总公司 | A kind of defoamer and its production and use |
CN106807122A (en) * | 2016-12-28 | 2017-06-09 | 广东中联邦精细化工有限公司 | A kind of phosphate fertilizer extraction production defoamer and preparation method thereof |
MX2021004621A (en) * | 2018-11-21 | 2021-07-07 | Dow Global Technologies Llc | Polyester foam control agents and methods of processing foodstuffs. |
CN113577833B (en) * | 2020-04-30 | 2023-05-05 | 江苏四新科技应用研究所股份有限公司 | Green solid defoaming agent and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1202386A (en) * | 1997-06-16 | 1998-12-23 | 杭州市化工研究所 | Compound defoamer and producing process |
EP1397188A1 (en) * | 2001-06-05 | 2004-03-17 | Basf Aktiengesellschaft | Defoaming agent and/or deaerating agent based on oil-in-water dispersions |
-
2005
- 2005-05-16 CN CNB2005100345830A patent/CN1326590C/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1202386A (en) * | 1997-06-16 | 1998-12-23 | 杭州市化工研究所 | Compound defoamer and producing process |
EP1397188A1 (en) * | 2001-06-05 | 2004-03-17 | Basf Aktiengesellschaft | Defoaming agent and/or deaerating agent based on oil-in-water dispersions |
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CN1721031A (en) | 2006-01-18 |
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