CNA - Improved preparation method of calcium dodecyl benzene sulfonate - Google Patents

Improved preparation method of calcium dodecyl benzene sulfonate Download PDF

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Publication number

CNA

CNA CN.1A CNA CNA CN A CN A CN A CN A CN A CN A CN A CN A CN A

Authority

CN

China

Prior art keywords

calcium

dodecylbenzene sulphonate

benzene sulfonate

sedimentation

dodecyl benzene

Prior art date

-12-28

Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)

Pending

Application number

CN.1A

Other languages

Chinese (zh)

Inventor

王怀恩

苏玉清

薛金枝

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

TIANJIN TIANCHUAN CHEMICAL CO Ltd

Original Assignee

TIANJIN TIANCHUAN CHEMICAL CO Ltd

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

-12-28

Filing date

-12-28

Publication date

-07-01

-12-28 Application filed by TIANJIN TIANCHUAN CHEMICAL CO Ltd filed Critical TIANJIN TIANCHUAN CHEMICAL CO Ltd

-12-28 Priority to CN.1A priority Critical patent/CNA/en

-07-01 Publication of CNA publication Critical patent/CNA/en

Status Pending legal-status Critical Current

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• preparation method Methods 0.000 title claims abstract description 15
• OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 title abstract 6
• sedimentation Methods 0.000 claims abstract description 25
• solvent Substances 0.000 claims abstract description 14
• liquid Substances 0.000 claims abstract description 9
• sediment Substances 0.000 claims abstract description 9
• VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 8
• method Methods 0.000 claims abstract description 8
• stirring Methods 0.000 claims abstract description 8
• suction filtration Methods 0.000 claims abstract description 6
• AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 5
• calcium hydroxide Substances 0.000 claims abstract description 5
• calcium hydroxide Inorganic materials 0.000 claims abstract description 5
• neutralization reaction Methods 0.000 claims abstract description 5
• XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
• calcium carbonate Inorganic materials 0.000 claims abstract description 4
• OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
• HCWYXKWQOMTBKY-UHFFFAOYSA-N calcium;dodecyl benzenesulfonate Chemical compound [Ca].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 HCWYXKWQOMTBKY-UHFFFAOYSA-N 0.000 claims description 27
• solution Substances 0.000 claims description 14
• chemical reaction Methods 0.000 claims description 13
• concentrate Substances 0.000 claims description 7
• vacuum filtration Methods 0.000 claims description 6
• acid Substances 0.000 claims description 5
• dilution Methods 0.000 claims description 4
• dilution Substances 0.000 claims description 4
• mother liquor Substances 0.000 claims description 4
• biosynthetic process Effects 0.000 claims description 3
• diluting agent Substances 0.000 claims description 3
• synthesis reaction Methods 0.000 claims description 3
• filtration Methods 0.000 abstract description 7
• energy consumption Methods 0.000 abstract description 4
• waste material Substances 0.000 abstract description 4
• chemical reaction liquid Substances 0.000 abstract 3
• WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 abstract 1
• cyclic group Chemical group 0.000 abstract 1
• diluting Methods 0.000 abstract 1
• dodecylbenzenesulfonic acid Drugs 0.000 abstract 1
• VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
• engineering process Methods 0.000 description 3
• beneficial effect Effects 0.000 description 2
• emulsion Substances 0.000 description 2
• modification Effects 0.000 description 2
• modification Methods 0.000 description 2
• sludge Substances 0.000 description 2
• sorption measurement Methods 0.000 description 2
• agitation Methods 0.000 description 1
• anionic surfactant Substances 0.000 description 1
• crystal Substances 0.000 description 1
• inorganic salt Inorganic materials 0.000 description 1
• inorganic solvent Inorganic materials 0.000 description 1
• mixing Methods 0.000 description 1
• precipitation Methods 0.000 description 1
• reaction time Effects 0.000 description 1
• solvate Substances 0.000 description 1
• substance Substances 0.000 description 1

Landscapes

• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention provides an improved preparation method of calcium dodecyl benzene sulfonate. The method comprises a neutralization reaction between dodecylbenzene sulfonic acid and calcium hydroxide or calcium carbonate and treatment on the reaction liquid generating calcium dodecyl benzene sulfonate. The improvement is that the treatment on the reaction liquid generating calcium dodecyl benzene sulfonate comprises the following steps: firstly driving the reaction liquid into a sedimentation kettle with a stirring function, and standing for 10-15 hours; putting the upper-layer liquid in the sedimentation kettle into a concentration kettle, and concentrating to remove solvents and little water to obtain a finished product of calcium dodecyl benzene sulfonate; adding a solvent into the lower-layer sediment in the sedimentation kettle, and stirring and diluting; driving the dilute liquid in the sedimentation kettle into a filter tank, and performing vacuum suction filtration; pouring the mother liquid after the suction filtration into a storage tank for cyclic utilization to synthesize calcium dodecyl benzene sulfonate; and burning the filter residue after the vacuum suction filtration. The method has the functions of facilitating filtration, increasing the product yield and reducing the energy consumption and waste residue discharge.

Description

The preparation method of the calcium dodecylbenzene sulphonate improved Background technology Calcium dodecylbenzene sulphonate is a kind of important anion surfactant, mainly for the preparation of farm chemical emulgent. Existing preparation method is, Witco Soft Acid and calcium hydroxide or calcium carbonate are reacted in methanol solvate, generate the solution of calcium dodecylbenzene sulphonate, this solution filters through plate-and-frame filter press, after mother liquor by dewatering precipitation, obtain calcium dodecylbenzene sulphonate finished product. The shortcoming that this preparation technology exists is, because the reaction solution viscosity generating calcium dodecylbenzene sulphonate is high, bad filtration, filter press is adopted to need a large amount of diatomite, and diatomite adsorption product, cause product yield to reduce, and cause filtration time long, energy consumption is high, the problem such as filter residue increase in discharge. Summary of the invention Main purpose of the present invention is the above-mentioned shortcoming overcoming currently available products existence, and a kind of preparation method of calcium dodecylbenzene sulphonate of improvement is provided, the post-treating method of preparation technology improved, is beneficial to filtration, improve product yield, reduce energy consumption, reduce waste sludge discharge. The object of the invention is to be realized by following technical scheme. The preparation method of the calcium dodecylbenzene sulphonate that the present invention improves, comprises the neutralization reaction of Witco Soft Acid and calcium hydroxide or calcium carbonate and generates the process of calcium dodecylbenzene sulphonate reaction solution; It is characterized in that, the process of the reaction solution of described generation calcium dodecylbenzene sulphonate is, is first beaten by reaction solution in the sedimentation still of band stirring, leaves standstill 10 to 15 hours; In sedimentation still, upper liquid puts concentrate to concentrate still, sloughs the water of solvent and trace, collects obtained calcium dodecylbenzene sulphonate finished product; In the lower floor's sediment in sedimentation still, add stirring solvent dilution, then the diluent in sedimentation still is squeezed into filter vat, carry out vacuum filtration; Mother liquor after suction filtration is poured in storage tank, is cycled to used in the synthesis of calcium dodecylbenzene sulphonate, the filter residue burning disposal after vacuum filtration. The preparation method of the calcium dodecylbenzene sulphonate of aforesaid improvement, wherein, the partial solvent that in described sedimentation still, upper liquid is sloughed in concentrate still is methyl alcohol; The described solvent added in the lower floor's sediment in sedimentation still is methyl alcohol, and the add-on of this methyl alcohol is 3 to 4 times of the lower floor's sediment weight in sedimentation still. Preparation method's beneficial effect of the calcium dodecylbenzene sulphonate that the present invention improves, improves the post-treating method of calcium dodecylbenzene sulphonate reaction solution, simplifies the operation, and shortens reaction time, improves product yield, reduces waste sludge discharge. Embodiment Embodiment: In L reactor, drop into quantitative methyl alcohol kg, Witco Soft Acid kg, after mixing, under stirring, add 170kg calcium hydroxide, control reaction solution pH value 7 to 8, temperature was 30 to 40 DEG C of reactions 1 hour, after reaction, reaction solution is beaten in the sedimentation still of band stirring, leave standstill 10 to 15 hours; In sedimentation still, upper strata emulsion is as clear as crystal shape, and this upper strata emulsion is put in concentrate still by sedimentation still side mouth, sloughs water and part methyl alcohol, the calcium dodecylbenzene sulphonate finished product of obtained about kg massfraction 65%; In a small amount of sediment of the lower floor in sedimentation still, add methyl alcohol be about L agitation and dilution, then the diluent in sedimentation still is squeezed into filter vat, carry out vacuum filtration, the mother liquor after suction filtration is poured in storage tank, is cycled to used in the synthesis of calcium dodecylbenzene sulphonate. Product yield reaches 90%, and comparatively prior art improves about 4 to 5%.The filter residue filtered is not containing diatomite, and filter residue output capacity declines 30%, and filter residue carries out doing burning disposal. The preparation method of the calcium dodecylbenzene sulphonate improved has the following advantages: 1, in the reacted sedimentation liquid of calcium dodecylbenzene sulphonate, 3 to 5 times of solvents are added, the concentration of calcium dodecylbenzene sulphonate in diluted settlement liquid, do not need during vacuum filtration to add diatomite, waste residue output capacity can be reduced, overcome again sediment viscosity large, the problem of sad filter, shortens filtration time, reduces energy consumption. Do not use diatomite when 2, filtering, the filter residue of filtration, only containing inorganic salt and solvent, is avoided diatomite adsorption product calcium dodecylbenzene sulphonate, is effectively improved product yield. 3, in Witco Soft Acid neutralization reaction, generation has water, the solvent that dilution is filtered afterwards contains micro-moisture (< 1%), solvent containing micro-moisture without impact, and can accelerate reaction solution settling velocity to neutralization reaction, shortens the sedimentation cycle. The above, it is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.

Claims (2)

1. a preparation method for the calcium dodecylbenzene sulphonate improved, comprises the neutralization reaction of Witco Soft Acid and calcium hydroxide or calcium carbonate and generates the process of calcium dodecylbenzene sulphonate reaction solution; It is characterized in that, the process of the reaction solution of described generation calcium dodecylbenzene sulphonate is, is first beaten by reaction solution in the sedimentation still of band stirring, leaves standstill 10 to 15 hours; In sedimentation still, upper liquid puts concentrate to concentrate still, sloughs the water of solvent and trace, collects obtained calcium dodecylbenzene sulphonate finished product; In the lower floor's sediment in sedimentation still, add stirring solvent dilution, then the diluent in sedimentation still is squeezed into filter vat, carry out vacuum filtration; Mother liquor after suction filtration is poured in storage tank, is cycled to used in the synthesis of calcium dodecylbenzene sulphonate, the filter residue burning disposal after vacuum filtration. 2. the preparation method of the calcium dodecylbenzene sulphonate of improvement according to claim 1, is characterized in that, the partial solvent that in described sedimentation still, upper liquid is sloughed in concentrate still is methyl alcohol; The described solvent added in the lower floor's sediment in sedimentation still is methyl alcohol, and the add-on of this methyl alcohol is 3 to 4 times of the lower floor's sediment weight in sedimentation still. CN.1A -12-28 -12-28 Improved preparation method of calcium dodecyl benzene sulfonate Pending CNA (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title CN.1A CNA (en) -12-28 -12-28 Improved preparation method of calcium dodecyl benzene sulfonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title CN.1A CNA (en) -12-28 -12-28 Improved preparation method of calcium dodecyl benzene sulfonate

Publications (1)

Publication Number Publication Date CNA true CNA (en) -07-01

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Application Number Title Priority Date Filing Date CN.1A Pending CNA (en) -12-28 -12-28 Improved preparation method of calcium dodecyl benzene sulfonate

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Cited By (4)

* Cited by examiner, † Cited by third party Publication number Priority date Publication date Assignee Title CNA (en) * -06-29 -10-08 无锡颐景丰科技有限公司 Method for directly preparing anhydrous calcium dodecyl benzene sulfonate and product CNA (en) * -08-26 -05-09 山东天道生物工程有限公司 Calcium dodecyl benzene sulfonate and preparation method thereof KRA (en) * -01-14 -07-21 주식회사 케미다스 Method for preparing alkali earth metal salt of alkylaryl sulfonic acid CNA (en) * -08-11 -11-14 安徽金桐精细化学有限公司 Preparation method of calcium dodecyl benzene sulfonate

• • -12-28 CN CN.1A patent/CNA/en active Pending

Cited By (6)

* Cited by examiner, † Cited by third party Publication number Priority date Publication date Assignee Title CNA (en) * -06-29 -10-08 无锡颐景丰科技有限公司 Method for directly preparing anhydrous calcium dodecyl benzene sulfonate and product KRA (en) * -01-14 -07-21 주식회사 케미다스 Method for preparing alkali earth metal salt of alkylaryl sulfonic acid KRB1 (en) -01-14 -02-20 주식회사 케미다스 Method for preparing alkali earth metal salt of alkylaryl sulfonic acid CNA (en) * -08-26 -05-09 山东天道生物工程有限公司 Calcium dodecyl benzene sulfonate and preparation method thereof CNB (en) * -08-26 -07-09 山东天道生物工程有限公司 Calcium dodecyl benzene sulfonate and preparation method thereof CNA (en) * -08-11 -11-14 安徽金桐精细化学有限公司 Preparation method of calcium dodecyl benzene sulfonate

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