CN204490770U - A kind of naphthalene continuous catalysis xanthator - Google Patents

A kind of naphthalene continuous catalysis xanthator Download PDF

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Publication number
CN204490770U
CN204490770U CN201520111507.4U CN201520111507U CN204490770U CN 204490770 U CN204490770 U CN 204490770U CN 201520111507 U CN201520111507 U CN 201520111507U CN 204490770 U CN204490770 U CN 204490770U
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sulfonation reaction
level
reaction still
mixing kettle
raw
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罗国林
冯辉
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Many Synthesis Chemical Co Ltds In Qujing
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Many Synthesis Chemical Co Ltds In Qujing
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Abstract

The naphthalene continuous catalysis xanthator that the utility model provides, be applicable to naphthalene continuous catalytic reaction, raw material sulphuric acid and melting refined naphthalene are tentatively mixed at one-level raw material mixing kettle, then fully mixed in secondary raw materials mixing kettle, order enters one-level sulfonation reaction still afterwards, secondary sulfonation reaction still, three grades of sulfonation reaction stills and level Four sulfonation reaction still carry out continuous sulfonation reaction, adopt the utility model as the device of sulfonation reaction, effectively decrease the consumption of raw material sulphuric acid, compared with traditional technology, sulfuric acid dosage reduces about 10%, the content of sulfonation reaction product Free Acid declines, thus effectively reduce the consumption of alkali and the generation of sodium sulfate byproduct in follow-up neutralization reaction, effectively decrease wastewater treatment load.In the production technique that the utility model provides simultaneously, factory effluent obtains effective recycle, has good economic benefit and environmental benefit, reduces enterprise cost and drops into, realize the production requirement of energy-saving and emission-reduction, environmental protection.

Description

A kind of naphthalene continuous catalysis xanthator
Technical field
The utility model belongs to naphthene sulfonic acid production technical field, is specifically related to a kind of naphthalene continuous catalysis xanthator.
Background technology
Beta-naphthalenesulfonic-acid is the important intermediate being used as to produce dyestuff, agricultural chemicals and medicine, is be that raw material obtains through sulfonation reaction with naphthalene.At present, in domestic and international industrial production, mostly adopt the excessive vitriol oil directly to carry out sulfonation reaction with melting naphthalene, because sulfuric acid consumption during sulfonation reaction is comparatively large, cause production cost input higher; The yield of target product beta-naphthalenesulfonic-acid is lower, is generally 64% ~ 66%(external standard method), 78% ~ 82%(HPLC); The content of by product is high, and is difficult to effectively separate from sulfonation reaction mixture, brings the difficulty that cannot overcome to follow-up workshop section; Such as in follow-up and the S-WAT that consumes of workshop section comparatively large, can produce a large amount of high salt organic waste waters, and a large amount of sulfur dioxide gas, cause the seriously corroded of equipment pipe, environmental pollution is larger.
Due to the restriction of above-mentioned sulfonating reaction process, cause the production cost of enterprise higher, and be difficult to the productive target realizing energy-saving and emission-reduction, clean environment firendly.
Utility model content
The purpose of this utility model is to provide a kind of naphthalene continuous catalysis xanthator.
The purpose of this utility model realizes like this, comprise catalyst carrier, sulfuric acid storage tank, sulfuric acid transferpump, well heater, refined naphthalene storage tank, refined naphthalene transferpump, raw material mixing kettle, sulfonation reaction still, steam condenser and condensate draining, described raw material mixing kettle comprises one-level raw material mixing kettle and secondary raw materials mixing kettle, described sulfonation reaction still comprises one-level sulfonation reaction still, secondary sulfonation reaction still, three grades of sulfonation reaction stills and level Four sulfonation reaction still, described catalyst carrier is connected with sulfuric acid storage tank, described sulfuric acid storage tank is connected with sulfuric acid transferpump, described sulfuric acid transferpump is linked in sequence one-level sulfuric acid well heater, be connected with one-level raw material mixing kettle after secondary sulfuric acid well heater, described refined naphthalene storage tank is connected with refined naphthalene transferpump, and described refined naphthalene transferpump is connected with one-level raw material mixing kettle after connecting refined naphthalene well heater, the discharge port of described one-level raw material mixing kettle is connected with the opening for feed of secondary raw materials mixing kettle, the discharge port of described secondary raw materials mixing kettle is connected with the opening for feed of one-level sulfonation reaction still, the discharge port of described one-level sulfonation reaction still is connected with the opening for feed of secondary sulfonation reaction still, the discharge port of described secondary sulfonation reaction still is connected with the opening for feed of three grades of sulfonation reaction stills, the discharge port of described three grades of sulfonation reaction stills is connected with the opening for feed of level Four sulfonation reaction still, and the discharge port of described level Four sulfonation reaction still is connected with the opening for feed of hydrolytic reaction pot, described one-level raw material mixing kettle, secondary raw materials mixing kettle, one-level sulfonation reaction still, secondary sulfonation reaction still, three grades of sulfonation reaction stills are connected with the inlet mouth of steam condenser with the air outlet, top of level Four sulfonation reaction still, and described steam condenser is connected with condensate draining.
The naphthalene continuous catalysis xanthator that the utility model provides, be applicable to naphthalene continuous catalytic reaction, raw material sulphuric acid and melting refined naphthalene are tentatively mixed at one-level raw material mixing kettle, then fully mixed in secondary raw materials mixing kettle, order enters one-level sulfonation reaction still afterwards, secondary sulfonation reaction still, three grades of sulfonation reaction stills and level Four sulfonation reaction still carry out continuous sulfonation reaction, adopt the utility model as the device of sulfonation reaction, effectively decrease the consumption of raw material sulphuric acid, compared with traditional technology, sulfuric acid dosage reduces about 10%, the content of sulfonation reaction product Free Acid declines, thus effectively reduce the consumption of alkali and the generation of sodium sulfate byproduct in follow-up neutralization reaction, effectively decrease wastewater treatment load.In the production technique that the utility model provides simultaneously, factory effluent obtains effective recycle, has good economic benefit and environmental benefit, reduces enterprise cost and drops into, realize the production requirement of energy-saving and emission-reduction, environmental protection.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
In figure: 1-catalyst carrier, 2-sulfuric acid storage tank, 3-sulfuric acid transferpump, 4-one-level sulfuric acid well heater, 5-secondary sulfuric acid well heater, 6-refined naphthalene storage tank, 7-refined naphthalene transferpump, 8-refined naphthalene well heater, 9-one-level raw material mixing kettle, 10-secondary raw materials mixing kettle, 11-one-level sulfonation reaction still, 12-secondary sulfonation reaction still, 13-tri-grades of sulfonation reaction stills, 14-level Four sulfonation reaction still, 15-hydrolytic reaction pot, 16-steam condenser, 17-condensate draining.
Embodiment
Be further described the utility model below in conjunction with drawings and Examples, but limited the utility model never in any form, any change done based on the utility model training centre or improvement, all belong to protection domain of the present utility model.
As shown in Figure 1, the naphthalene continuous catalysis xanthator that the utility model provides, comprise catalyst carrier 1, sulfuric acid storage tank 2, sulfuric acid transferpump 3, well heater, refined naphthalene storage tank 6, refined naphthalene transferpump 7, raw material mixing kettle, sulfonation reaction still, steam condenser 16 and condensate draining 17, described raw material mixing kettle comprises one-level raw material mixing kettle 9 and secondary raw materials mixing kettle 10, described sulfonation reaction still comprises one-level sulfonation reaction still 11, secondary sulfonation reaction still 12, three grades of sulfonation reaction stills 13 and level Four sulfonation reaction still 14, described catalyst carrier 1 is connected with sulfuric acid storage tank 2, described sulfuric acid storage tank 2 is connected with sulfuric acid transferpump 3, described sulfuric acid transferpump 3 is linked in sequence one-level sulfuric acid well heater 4, be connected with one-level raw material mixing kettle 9 after secondary sulfuric acid well heater 5, described refined naphthalene storage tank 6 is connected with refined naphthalene transferpump 7, and described refined naphthalene transferpump 7 is connected with one-level raw material mixing kettle 9 after connecting refined naphthalene well heater 8, the discharge port of described one-level raw material mixing kettle 9 is connected with the opening for feed of secondary raw materials mixing kettle 10, the discharge port of described secondary raw materials mixing kettle 10 is connected with the opening for feed of one-level sulfonation reaction still 11, the discharge port of described one-level sulfonation reaction still 11 is connected with the opening for feed of secondary sulfonation reaction still 12, the discharge port of described secondary sulfonation reaction still 12 is connected with the opening for feed of three grades of sulfonation reaction stills (13), the discharge port of described three grades of sulfonation reaction stills 13 is connected with the opening for feed of level Four sulfonation reaction still 14, the discharge port of described level Four sulfonation reaction still 14 is connected with the opening for feed of hydrolytic reaction pot 15, described one-level raw material mixing kettle 9, secondary raw materials mixing kettle 10, one-level sulfonation reaction still 11, secondary sulfonation reaction still 12, three grades of sulfonation reaction stills 13 are connected with the inlet mouth of steam condenser 16 with the air outlet, top of level Four sulfonation reaction still 14, and described steam condenser 16 is connected with condensate draining 17.
Described one-level sulfonation reaction still 11, secondary sulfonation reaction still 12, three grades of sulfonation reaction stills 13 and level Four sulfonation reaction still 14 are all with agitating function.
embodiment
The catalyzer of sulfuric acid total amount 5% is incorporated as in 98% sulfuric acid, the catalyzer added in described 98% sulfuric acid is prepared according to the following weight ratio, by sulfonated kerosene: NMP: trioctylamine: anhydrous sodium sulphate: naphthane joins in the preparation still of band agitating function by the weight ratio of 30:2:6:5:20, the temperature in preparation still is kept to be 30 DEG C, stir 60min, obtain catalyzer; Then 98% sulfuric acid containing catalyzer is sent into after one-level is heated to 45 DEG C secondary heating, secondary sends into one-level raw material mixing kettle 9 after being heated to 100 DEG C; Melting refined naphthalene sends into one-level raw material mixing kettle 9 after one-level is heated to 120 DEG C, 98% sulfuric acid in described feeding one-level raw material mixing kettle 9 and the mass ratio of refined naphthalene are 1:1.308,98% sulfuric acid containing catalyzer and melting refined naphthalene are sent into secondary raw materials mixing kettle 10 after preliminary mixing and are fully mixed in one-level raw material mixing kettle 9, and the mixing temperature in described one-level raw material mixing kettle 9 and secondary raw materials mixing kettle 10 is 160 DEG C; One-level sulfonation reaction still 11 sent into by material after mixing in secondary raw materials mixing kettle 10, after above-mentioned material reacts 60min in one-level sulfonation reaction still 11, the material in one-level sulfonation reaction still 11 sent into secondary sulfonation reaction still 12; After above-mentioned material reacts 60min in secondary sulfonation reaction still 12, the material in secondary sulfonation reaction still 12 is sent into three grades of sulfonation reaction stills 13; After above-mentioned material reacts 60min in three grades of sulfonation reaction stills 13, the material in three grades of sulfonation reaction stills 13 is sent into level Four sulfonation reaction still 14, above-mentioned material reacts 60min and completes sulfonation reaction in level Four sulfonation reaction still 14; Sulfonation reaction temperature in above-mentioned sulfonation reaction still at different levels is 162 DEG C, after sulfonation reaction terminates, and in products therefrom, the total reaction yield of beta-naphthalenesulfonic-acid is 81.2%(external standard method), 97.5%(HPLC).
The naphthalene continuous catalysis xanthator that the utility model provides has good expansibility, namely realizes expanding by increase and decrease sulfonation progression and supporting xanthator; In actual production process, can according to the reaction yield requirement of actual beta-naphthalenesulfonic-acid, increase and decrease sulfonation reaction progression, thus effective cost-saving input.

Claims (2)

1. one kind is applicable to the device of naphthalene continuous catalysis method of sulfonating, comprise catalyst carrier (1), sulfuric acid storage tank (2), sulfuric acid transferpump (3), well heater, refined naphthalene storage tank (6), refined naphthalene transferpump (7), raw material mixing kettle, sulfonation reaction still, steam condenser (16) and condensate draining (17), described raw material mixing kettle comprises one-level raw material mixing kettle (9) and secondary raw materials mixing kettle (10), described sulfonation reaction still comprises one-level sulfonation reaction still (11), secondary sulfonation reaction still (12), three grades of sulfonation reaction stills (13) and level Four sulfonation reaction still (14), it is characterized in that described catalyst carrier (1) is connected with sulfuric acid storage tank (2), described sulfuric acid storage tank (2) is connected with sulfuric acid transferpump (3), described sulfuric acid transferpump (3) is linked in sequence one-level sulfuric acid well heater (4), secondary sulfuric acid well heater (5) is connected with one-level raw material mixing kettle (9) afterwards, described refined naphthalene storage tank (6) is connected with refined naphthalene transferpump (7), and described refined naphthalene transferpump (7) connects refined naphthalene well heater (8) and is connected with one-level raw material mixing kettle (9) afterwards, the discharge port of described one-level raw material mixing kettle (9) is connected with the opening for feed of secondary raw materials mixing kettle (10), the discharge port of described secondary raw materials mixing kettle (10) is connected with the opening for feed of one-level sulfonation reaction still (11), the discharge port of described one-level sulfonation reaction still (11) is connected with the opening for feed of secondary sulfonation reaction still (12), the discharge port of described secondary sulfonation reaction still (12) is connected with the opening for feed of three grades of sulfonation reaction stills (13), the discharge port of described three grades of sulfonation reaction stills (13) is connected with the opening for feed of level Four sulfonation reaction still (14), the discharge port of described level Four sulfonation reaction still (14) is connected with the opening for feed of hydrolytic reaction pot (15), described one-level raw material mixing kettle (9), secondary raw materials mixing kettle (10), one-level sulfonation reaction still (11), secondary sulfonation reaction still (12), three grades of sulfonation reaction stills (13) are connected with the inlet mouth of steam condenser (16) with the air outlet, top of level Four sulfonation reaction still (14), and described steam condenser (16) is connected with condensate draining (17).
2. device according to claim 1, is characterized in that described one-level sulfonation reaction still (11), secondary sulfonation reaction still (12), three grades of sulfonation reaction stills (13) and level Four sulfonation reaction still (14) are all with agitating function.
CN201520111507.4U 2015-02-16 2015-02-16 A kind of naphthalene continuous catalysis xanthator Active CN204490770U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003070A (en) * 2017-12-22 2018-05-08 绍兴杰派化工科技有限公司 A kind of method of sulfonation in H acid production
CN108822006A (en) * 2018-05-31 2018-11-16 山西豪仑科化工有限公司 A kind of naphthalene sulfonation continuous reaction process

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003070A (en) * 2017-12-22 2018-05-08 绍兴杰派化工科技有限公司 A kind of method of sulfonation in H acid production
CN108822006A (en) * 2018-05-31 2018-11-16 山西豪仑科化工有限公司 A kind of naphthalene sulfonation continuous reaction process

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