CN108129359A - A kind of preparation method of phosphoric acid extraction antifoaming agent - Google Patents
A kind of preparation method of phosphoric acid extraction antifoaming agent Download PDFInfo
- Publication number
- CN108129359A CN108129359A CN201711188124.7A CN201711188124A CN108129359A CN 108129359 A CN108129359 A CN 108129359A CN 201711188124 A CN201711188124 A CN 201711188124A CN 108129359 A CN108129359 A CN 108129359A
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- CN
- China
- Prior art keywords
- phosphoric acid
- esterification
- acid extraction
- product
- antifoaming agent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation methods of phosphoric acid extraction antifoaming agent, and esterification and process for sulfonation are completed using one pot, it is characterised in that：1) esterification by mass fraction be 20~27% maleic anhydride, 70~77% isooctanol and 1~3% p-methyl benzenesulfonic acid, it it is 90~120 DEG C in temperature, pressure is to be reacted 3-6 hours under 0.08~0.1MPa, obtains esterification reaction product diisooctyl maleate；2) sulfonating reaction is 40~50% esterification reaction product diisooctyl maleates, 5~20% diisooctyl succinate sodium sulfonates, 10~15% sodium pyrosulfites and 25~35% water by mass fraction, it is 100~105 DEG C, reacted 5~8 hours under normal pressure that products therefrom is that the liquid of homogeneous phase transparent is phosphoric acid extraction antifoaming agent in temperature.The present invention has easy to operate, and by-product is few, and obtains anti-foam product homogeneous, that color is shallow.The product shows as the characteristics of dosage is few, antifoaming speed is fast, the suds time is long when being applied in phosphoric acid extraction.
Description
Technical field
The present invention relates to a kind of preparation methods of phosphoric acid extraction antifoaming agent, belong to phosphoric acid preparing technical field.
Background technology
In Wet-process Phosphoric Acid Production, the carbonate in rock phosphate in powder reacts with acid generates a large amount of CO2Gas.With acidolysis
The fierce of process carries out, CO2Continuously be dispersed in the reaction solution containing organic components, formed on slurry surface one it is stable
Froth bed brings phosphoric acid by wet process many adverse effects.
First, dispersion and the acidolysis reaction of phosphate ore pulp are influenced, production capacity is caused to decline；Secondly, froth bed both reduced
The utilization rate of equipment, and make material position observation difficult；Third hinders reaction temperature raising, and foam can be by a large amount of bands extremely when serious
The even unrestrained slot of tail gas absorbing system, causes P2O5Loss and environmental pollution.
The product colour that existing defoaming agent producing process obtains is deeper, and by-product is more；Sulfonating reaction product is non-equal
Phase system need to separate raw material of the water phase as next secondary response, not only cumbersome in this way, but also be unfavorable for the steady of product quality
It is fixed.
Invention content
The purpose of the present invention is deeper in order to overcome the product colour that existing defoaming agent producing process obtains, and by-product is more；
Sulfonating reaction product is heterogeneous system, and provides a kind of preparation method of phosphoric acid extraction antifoaming agent, production technology of the invention
It is easy to operate, the obtained product liquid shallow for homogeneous, color.The product shows as that dosage is few, disappears when being applied in phosphoric acid extraction
Bubble speed is fast, the suds time is long.
The technical scheme is that：
A kind of preparation method of phosphoric acid extraction antifoaming agent completes esterification and process for sulfonation using one pot, it is characterised in that：
1) esterification is by maleic anhydride of the mass fraction for 20~27%, 70~77% isooctanol and 1~3%
P-methyl benzenesulfonic acid, temperature be 90~120 DEG C, pressure be -0.08~-0.1MPa under react 3-6 hour, obtain be esterified instead
Answer product diisooctyl maleate.
2) sulfonating reaction is 40~50% esterification reaction product diisooctyl maleates, 5~20% by mass fraction
Diisooctyl succinate sodium sulfonate, 10~15% sodium pyrosulfites and 25~35% water are 100~105 DEG C, under normal pressure in temperature
Reaction 5~8 hours, products therefrom is that the liquid of homogeneous phase transparent is phosphoric acid extraction antifoaming agent.
Advantageous effect：The simple in production process operation of the present invention, the obtained product liquid shallow for homogeneous, color.The product
Show as that dosage is few, antifoaming speed is fast, the suds time is long when being applied in phosphoric acid extraction.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
Esterification is 120 in temperature by 1.4kg maleic anhydrides, 5.3kg isooctanol and 0.2kg p-methyl benzenesulfonic acid
DEG C, pressure is to be reacted 3 hours under -0.1MPa；Obtain 6.6kg esterification reaction product diisooctyl maleates；
Sulfonating reaction is by 6.6kg esterification reaction products diisooctyl maleate, 1.6kg succinic acid di-isooctyl sulfonic acid
The water of sodium, 1.8kg sodium pyrosulfites and 3.8kg is 105 DEG C, is reacted 6 hours under normal pressure that products therefrom is homogeneous saturating in temperature
Bright liquid is phosphoric acid extraction antifoaming agent.
In phosphoric acid extraction technique, this product is pressed to the speed of 2.55kg/h, puts into 25.5 tons of P2O5The phosphoric acid extraction dress of/h
In putting, in 37 seconds, all foams all eliminate, and just start new foam occur after 6 minutes.
Embodiment 2
Esterification is 120 in temperature by 1075kg maleic anhydrides, 2890kg isooctanol and 40kg p-methyl benzenesulfonic acid
DEG C, pressure is to be reacted 5 hours under -0.095MPa, obtains 3820kg esterification reaction product diisooctyl maleates；
Sulfonating reaction is by 3820kg esterification reaction products diisooctyl maleate, 1300kg succinic acid di-isooctyl sulphurs
The water of sour sodium, 1400kg sodium pyrosulfites and 3000kg is 103 DEG C, is reacted 8 hours under normal pressure that products therefrom is equal in temperature
Mutually transparent liquid is phosphoric acid extraction antifoaming agent.
In phosphoric acid extraction technique, this product is pressed to the speed of 5.1kg/h, puts into 25.5 tons of P2O5The phosphoric acid extraction dress of/h
In putting, in 28 seconds, all foams all eliminate, and just start new foam occur after 13 minutes.
Embodiment 3
Esterification is 120 in temperature by 2.1kg maleic anhydrides, 6.3kg isooctanol and 0.1kg p-methyl benzenesulfonic acid
DEG C, pressure is to be reacted 3 hours under -0.1MPa；Obtain the esterification reaction product diisooctyl maleate of 8.1kg；
Sulfonating reaction is by 8.1kg esterification reaction products diisooctyl maleate, 1.1kg succinic acid di-isooctyl sulfonic acid
The water of sodium, 2.1kg sodium pyrosulfites and 5.4kg is 105 DEG C, is reacted 5 hours under normal pressure that gained 16.7kg products are in temperature
The liquid of homogeneous phase transparent is phosphoric acid extraction antifoaming agent.
In phosphoric acid extraction technique, this product is pressed to the speed of 7.65kg/h, puts into 25.5 tons of P2O5The phosphoric acid extraction dress of/h
In putting, in 20 seconds, all foams all eliminate, and just start new foam occur after 19 minutes.
Embodiment 4
Esterification is 90 in temperature by 820kg maleic anhydrides, 3068kg isooctanol and 112kg p-methyl benzenesulfonic acid
DEG C, pressure is to be reacted 6 hours under -0.1MPa；Obtain the esterification reaction product diisooctyl maleate of 3811.8kg；
Sulfonating reaction is different pungent by 3811.8kg esterification reaction products diisooctyl maleate, 1863.5kg succinic acid two
The water of ester sodium sulfonate, 950.6kg sodium pyrosulfites and 2785.9kg is 100 DEG C, is reacted 8 hours under normal pressure, gained in temperature
9411.8kg products are that the liquid of homogeneous phase transparent is phosphoric acid extraction antifoaming agent.
Claims (1)
1. a kind of preparation method of phosphoric acid extraction antifoaming agent completes esterification and process for sulfonation using one pot, it is characterised in that：
1) esterification：By maleic anhydride that mass fraction is 20~27%, 70~77% isooctanol and 1~3%
P-methyl benzenesulfonic acid is 90~120 DEG C in temperature, and pressure is to be reacted 3~6 hours under -0.08~-0.1MPa, obtains esterification
Product diisooctyl maleate.
2) sulfonating reaction：It is 40~50% esterification reaction product diisooctyl maleates by mass fraction, 5~20% fourths two
Sour di-isooctyl sodium sulfonate, 10~15% sodium pyrosulfites and 25~35% water are 100~105 DEG C, are reacted under normal pressure in temperature
5~8 hours, products therefrom was that the liquid of homogeneous phase transparent is phosphoric acid extraction antifoaming agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711188124.7A CN108129359A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of phosphoric acid extraction antifoaming agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711188124.7A CN108129359A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of phosphoric acid extraction antifoaming agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108129359A true CN108129359A (en) | 2018-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711188124.7A Pending CN108129359A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of phosphoric acid extraction antifoaming agent |
Country Status (1)
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| CN (1) | CN108129359A (en) |
Citations (8)
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|---|---|---|---|---|
| US4111903A (en) * | 1976-05-03 | 1978-09-05 | Tenneco Chemicals, Inc. | Organotin compounds and vinyl halide resin compositions stabilized therewith |
| US4470881A (en) * | 1981-03-23 | 1984-09-11 | Celanese Corporation | Separation of ethyl acetate from methyl ethyl ketone by extractive distillation |
| CN1160710A (en) * | 1996-03-25 | 1997-10-01 | 南京理工大学 | Preparation process of diisooctyl sodium sulfosuccinate |
| CN101284806A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Clean production process for sodium diethylhexyl sulfosuccinate |
| CN102391158A (en) * | 2011-08-04 | 2012-03-28 | 浙江合诚化学有限公司 | Preparation method of isooctanol polyoxypropylene ether sodium sulfosuccinate diester |
| CN103030966A (en) * | 2012-12-24 | 2013-04-10 | 建德市顺发化工助剂有限公司 | Preparation method of high-efficiency penetrant for PU synthetic leather |
| CN103709078A (en) * | 2013-12-31 | 2014-04-09 | 广州星业科技股份有限公司 | Preparation method of dioctyl sodium sulfosuccinate |
| CN104829503A (en) * | 2015-05-27 | 2015-08-12 | 北京康远制药有限公司 | Method for preparing high-purity docusate sodium |
-
2017
- 2017-11-24 CN CN201711188124.7A patent/CN108129359A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4111903A (en) * | 1976-05-03 | 1978-09-05 | Tenneco Chemicals, Inc. | Organotin compounds and vinyl halide resin compositions stabilized therewith |
| US4470881A (en) * | 1981-03-23 | 1984-09-11 | Celanese Corporation | Separation of ethyl acetate from methyl ethyl ketone by extractive distillation |
| CN1160710A (en) * | 1996-03-25 | 1997-10-01 | 南京理工大学 | Preparation process of diisooctyl sodium sulfosuccinate |
| CN101284806A (en) * | 2008-06-06 | 2008-10-15 | 江苏省海安石油化工厂 | Clean production process for sodium diethylhexyl sulfosuccinate |
| CN102391158A (en) * | 2011-08-04 | 2012-03-28 | 浙江合诚化学有限公司 | Preparation method of isooctanol polyoxypropylene ether sodium sulfosuccinate diester |
| CN103030966A (en) * | 2012-12-24 | 2013-04-10 | 建德市顺发化工助剂有限公司 | Preparation method of high-efficiency penetrant for PU synthetic leather |
| CN103709078A (en) * | 2013-12-31 | 2014-04-09 | 广州星业科技股份有限公司 | Preparation method of dioctyl sodium sulfosuccinate |
| CN104829503A (en) * | 2015-05-27 | 2015-08-12 | 北京康远制药有限公司 | Method for preparing high-purity docusate sodium |
Non-Patent Citations (2)
| Title |
|---|
| DAOHONG ZHANG ET AL: "Synthesis and Characterization of a Novel Low-Viscosity Unsaturated Hyperbranched Polyester Resin", 《CHEM. ENG. TECHNOL.》 * |
| 张万忠等: "琥珀酸二异辛酯磺酸钠制备的影响因素研究", 《化学试剂》 * |
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