CN101585675B - Sulphonation method for naphthalene series water reducing agent without naphthalene discharging - Google Patents
Sulphonation method for naphthalene series water reducing agent without naphthalene discharging Download PDFInfo
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- CN101585675B CN101585675B CN2009100334834A CN200910033483A CN101585675B CN 101585675 B CN101585675 B CN 101585675B CN 2009100334834 A CN2009100334834 A CN 2009100334834A CN 200910033483 A CN200910033483 A CN 200910033483A CN 101585675 B CN101585675 B CN 101585675B
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- naphthalene
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- sulphonation
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Abstract
The invention discloses a sulphonation method for a naphthalene series water reducing agent without naphthalene discharging, aiming at the defects in the synthesis technological process of the prior naphthalene series water reducing agent production by sulphonation-hydrolyzation-condensation-neutralisation. The sulphonation method comprises: feeding solvent to a reactor, dissolving the evaporated naphthalene, forming the naphthalene solution, vaporizing and condensing the naphthalene solution, separating the naphthalene solvent and the acid water by a oil-water separation system, feeding the naphthalene solution containing the naphthalene into a sulphonation reaction system in cycle, continuously sulfonating the naphthalene in the naphthalene solution, hydrolyzing, condensing and neutralizing to obtain the dry powder products, thus achieving the discharging without naphthalene and exhaust.
Description
Technical field
The present invention relates to the method for sulfonating of naphthalene water reducer, the especially naphthalene series water reducing agent without naphthalene discharging of cement concrete use.
Background technology
The naphthalene water reducer main chemical compositions is: the beta-naphthalenesulfonic-acid formaldehyde polymkeric substance.Naphthalene water reducer is that utilization is widest in area in the high efficiency water reducing agent, usage quantity is maximum at present, also is the maximum concrete admixture of turnout.According to incompletely statistics, nearly more than the 30 ten thousand tons of naphthalene water reducer pulvis of national YO, its working method comparative maturity adopts compound methods such as sulfonation, hydrolysis, condensation, neutralization to form.
But this method has major defect, in sulfonation process, because naphthalene has the physical property and the naphthalene method of sulfonating characteristics of distillation, thereby in sulfonation process, produces a large amount of naphthalene, water and SO
2Discharging.Mainly take at present bulky naphthalene sublimate receiving device and exhaust gas processing device; In the recycling process, the naphthalene material of sublimating contains the sour water that a large amount of sulfonation reaction generates, and the quality of product receives very big influence; And; Handle the back to the naphthalene of collecting and recycle, consumed the time, equipment and manpower, be unfavorable for the protection of environment.
Summary of the invention
The object of the invention is exactly the defective to former method, and a kind of method of sulfonating of new naphthalene series water reducing agent without naphthalene discharging is provided.
The present invention realizes through following technical scheme:
In sulfonation process, add solvent to reaction kettle, after the naphthalene dissolving with evaporation; Form naphthalene solution, naphthalene solution is after evaporation, condensation, through through oil-water separation system; After naphthalene solvent and sour water separation, contain the naphthalene solution of naphthalene, circulation is sent in the sulfonation reaction system; Naphthalene in the naphthalene solution constantly is sulfonated, and after hydrolysis, condensation, neutralization, obtains power-product again, has finally reached the purpose of no naphthalene, non-exhaust emission.
Used solvent is hexanaphthene, benzene, YLENE, benzene dichloride, tri-chlorination benzene, alkane, halohydrocarbon with and verivate and mixture in one or more compsn.
The method of the method that adopts for using solvent cycle or being interrupted filling, perhaps after the filling, after separator separates, row filling again in another one or more than one batch.
It is stable that the present invention has the feed ratio of product; Because the discharging of the nothing of naphthalene, the yield of product improves 2-3%; Improve the yield and the stability of product; Strengthen Enterprises'Competitiveness; Economize on resources; The protection mankind depend on for existence advantages such as environment.
Further set forth the present invention through instance below, but be not limited to the present invention.
Embodiment
Embodiment one:
Drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 3000KG at the 8000L enamel reaction still, heat up, open solvent pump simultaneously, add hexanaphthene; Control filling speed 10L/ minute is warming up to 130 ℃, adds vitriol oil 3700KG, sulfonation temperature 155-165 ℃; After 2 hours sulfonation time, close solvent pump, continue sulfonation one hour.After the hydrolysis of 20000L reaction kettle, condensation, after the neutralization spray is done, get 8.63 tons of power-products again.Each item index and the contrast of former method:
Embodiment two:
Drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 3000KG at the 8000L enamel reaction still, be warming up to 130 ℃, add vitriol oil 3700KG, open solvent pump simultaneously; Add benzene, control filling speed 60L/ minute, 10 minutes filling time, sulfonation 2 hours; Open solvent pump again, add benzene, control filling speed 60L/ minute; Annotate after 10 minutes, close solvent pump, continue sulfonation one hour.After the hydrolysis of 20000L reaction kettle, condensation, after the neutralization spray is done, get 8.58 tons of power-products again.Each item index and the contrast of former method:
Embodiment three:
Drop into NAPTHALENE FLAKES. (INDUSTRIAL GRADE 3000KG at the 8000L enamel reaction still, be warming up to 130 ℃, add vitriol oil 3700KG, open solvent pump simultaneously; The mixed solvent that adds benzene and hexanaphthene, control filling speed 60L/ minute, 10 minutes filling time, sulfonation is in the time of 2 hours; Open solvent pump again, add mixed solvent, control filling speed 60L/ minute; Annotated 10 minutes, and closed solvent pump, continue sulfonation one hour.After the hydrolysis of 20000L reaction kettle, condensation, after the neutralization spray is done, get 8.62 tons of power-products again.Each item index and the contrast of former method:
Claims (1)
1. the method for sulfonating of a naphthalene series water reducing agent without naphthalene discharging is characterized in that: in sulfonation process, add solvent to reaction kettle; The naphthalene dissolving back of evaporation is formed naphthalene solution, and naphthalene solution is after evaporation, condensation, through through oil-water separation system; To containing the naphthalene solution of naphthalene after naphthalene solvent and the sour water separation; Circulation is sent in the sulfonation reaction system, and the naphthalene in the naphthalene solution constantly is sulfonated, and after hydrolysis, condensation, neutralization, obtains power-product again; Finally reached the purpose of no naphthalene, non-exhaust emission, wherein used solvent is one or more the compsn in hexanaphthene, benzene, YLENE, benzene dichloride, the tri-chlorination benzene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100334834A CN101585675B (en) | 2009-06-22 | 2009-06-22 | Sulphonation method for naphthalene series water reducing agent without naphthalene discharging |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100334834A CN101585675B (en) | 2009-06-22 | 2009-06-22 | Sulphonation method for naphthalene series water reducing agent without naphthalene discharging |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101585675A CN101585675A (en) | 2009-11-25 |
| CN101585675B true CN101585675B (en) | 2012-05-23 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100334834A Expired - Fee Related CN101585675B (en) | 2009-06-22 | 2009-06-22 | Sulphonation method for naphthalene series water reducing agent without naphthalene discharging |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101797471B (en) * | 2010-04-16 | 2012-09-19 | 广西红墙新材料有限公司 | Treating and recycling method of tail gas generating in sulfonated naphthaldehyde water reducing agent production and special equipment |
| CN102746195A (en) * | 2011-04-27 | 2012-10-24 | 江苏尼高科技有限公司 | Method for improving sulfonation process of naphthalene-based water reducer |
| CN105884238B (en) * | 2015-08-18 | 2017-12-22 | 科之杰新材料集团有限公司 | A kind of naphthalene system pulvis water reducer and preparation method thereof |
| CN106117481B (en) * | 2016-06-24 | 2018-06-08 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the production method of sulfonation separate mealing type condensation production naphthalene water reducer |
| CN106082756B (en) * | 2016-06-24 | 2018-01-09 | 山东省莱芜市汶河化工有限公司 | A kind of solvent method concentrates the production system of sulfonation separate mealing type condensation production naphthalene water reducer |
| CN106146356B (en) * | 2016-07-01 | 2018-07-20 | 宁夏紫光川庆化工有限公司 | The method of continuous production 1-naphthalene sulfonic aicd |
| CN106396459A (en) * | 2016-08-30 | 2017-02-15 | 卓达新材料科技集团威海股份有限公司 | Efficient reducer for 3D printing house thick liquid |
| CN106632938B (en) * | 2016-09-20 | 2019-01-01 | 江苏苏博特新材料股份有限公司 | A kind of energy saving preparation method and its special equipment of naphthalene water reducer |
| CN110964160A (en) * | 2019-12-11 | 2020-04-07 | 广东科隆智谷新材料股份有限公司 | Method for preparing naphthalene water reducer by using waste sulfuric acid from nekal |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314556A (en) * | 2007-05-28 | 2008-12-03 | 重庆达华砼外加剂科技发展有限公司 | Process for recovering residual naphthalin in naphthalin series water reducing agent synthesis |
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- 2009-06-22 CN CN2009100334834A patent/CN101585675B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314556A (en) * | 2007-05-28 | 2008-12-03 | 重庆达华砼外加剂科技发展有限公司 | Process for recovering residual naphthalin in naphthalin series water reducing agent synthesis |
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| CN101585675A (en) | 2009-11-25 |
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