CN104974063A - Preparation method of sulfanilic acid by solid-phase process - Google Patents
Preparation method of sulfanilic acid by solid-phase process Download PDFInfo
- Publication number
- CN104974063A CN104974063A CN201510462711.5A CN201510462711A CN104974063A CN 104974063 A CN104974063 A CN 104974063A CN 201510462711 A CN201510462711 A CN 201510462711A CN 104974063 A CN104974063 A CN 104974063A
- Authority
- CN
- China
- Prior art keywords
- acid
- aniline
- sulphanilic acid
- crude product
- sulphanilic
- Prior art date
- 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
Links
- 0 N=CC1C=C*=CC1 Chemical compound N=CC1C=C*=CC1 0.000 description 2
- ATMSQOAHGUFOMY-MRVPVSSYSA-N C#C[C@@H]1CC=CCC1 Chemical compound C#C[C@@H]1CC=CCC1 ATMSQOAHGUFOMY-MRVPVSSYSA-N 0.000 description 1
- DFVNMKGXTHPRJM-UHFFFAOYSA-N C(C1)C1C1CC=CCC1 Chemical compound C(C1)C1C1CC=CCC1 DFVNMKGXTHPRJM-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of sulfanilic acid by a solid-phase process, which comprises the following steps: carrying out salification reaction on aniline and sulfuric acid to generate aniline sulfonate, sulfonating, baking to obtain a sulfanilic acid crude product, pulverizing the crude product, dissolving, carrying out vacuum filtration, crystallizing, centrifuging, dehydrating, and carrying out microwave drying to obtain the sulfanilic acid refined product. The preparation technique is simple, saves the aniline dropwise addition operation, shortens the salification reaction time, and lowers the material reaction temperature, energy consumption and waste gas emission. The process water in production is recycled, so no wastewater is discharged, thereby reducing the environmental pollution.
Description
Technical field
The present invention relates to a kind of production technique of Sulphanilic Acid, especially a kind of preparation method of Sulphanilic Acid solid phase method.
Background technology
Sulphanilic Acid is a kind of important intermediate being mainly used in dyestuff, dyeing and printing auxiliary, food color, spices, agricultural chemicals, and it can be used for producing Acid Orange II, acid brilliant yellow 2g, the yellowish-brown 4G of acidic intermedium, Acid Chrome Deep Yellow GG, direct yellow GR, reactive brilliant red k-2g and active purple k-3r etc.; Also can be used for the auxiliary agent in some product manufacturing, as Liovatin S, fluorescent brightening BG, BBU, dust-proof salt H etc., also can be used for agricultural bactericide, prevent wheat rust.In addition or the desirable feedstock of the industry such as medicine, building materials, as cement adds this product, setting time can not only be shortened, intensity can also be improved, increase the service life.In a word, this product is emerging chemical industry intermediate materials body, and of many uses, supply falls short of demand in the international market.Product finds a good sale in the countries and regions such as Switzerland, Germany, Indonesia, Brazil, Ah Gen the court of a feudal ruler, India.The big or middle enterprise of domestic small part also brings into use, and has good market outlook.
The basic principles of chemistry that Sulphanilic Acid is produced are completed by following two processes: (1) is by aniline and sulfuric acid generation salt-forming reaction; (2) anilinesulfonic acid salt is through dehydration, the obtained Sulphanilic Acid of molecular transposition (transposition).
At present, domestic enterprise mostly adopts conventional liquid phase method explained hereafter, but the quality product that liquid phase method technique obtains is poor, the production of fine chemical product can not be applied to, and processing to cure the time long, energy consumption is large, sulfide, aniline waste water and discharge amount of exhaust gas are many, contaminate environment, Chinese Patent Application No. 201310500142.X discloses a kind of preparation method of Sulphanilic Acid, and the method complete processing is too simple, and the operation time is long, the product water content of making is large, also has suitable difficulty for factorial praluction.
Summary of the invention
Therefore, people are to easy making process, there is great demand in the production technology of fast energy-saving environmental protection, up to now, also do not find the relevant report preparing Sulphanilic Acid about solid phase method of the present invention, the present inventor, through research trial repeatedly, finally successfully develops the preparation method of Sulphanilic Acid solid phase method, thus completes the present invention.
Object of the present invention is just to provide a kind of preparation method of Sulphanilic Acid solid phase method.
Accompanying drawing illustrates:
Fig. 1 is the solid phase method technological process of production and node control skeleton diagram.
The invention has the beneficial effects as follows that preparation technology is simple, effectively saves the dropwise operation of aniline and the reaction times of salify, reduces the temperature of reaction of material and the consumption of the energy, and waste gas, waste water discharge, decrease the pollution to environment.
Embodiment:
Technology of preparing scheme of the present invention is as follows, and it comprises the following steps:
1, salt-forming reaction: be first the sulfuric acid of 93% by levels, pump in high-order test tank with sulfuric acid pump, take 21.75 tons, sulfuric acid is added in sulfonation reaction still, with aniline pump, the aniline of levels 99% is pumped in the high-order test tank of aniline again, take 19.2 tons (aniline and sulfuric acid weight ratio are 1:1.1.33), open benzene peace test tank bottom valve, aniline is slowly dripped and adds in the sulfonation reaction still of sulfuric acid, after dripping, mixing and stirring, closed reactor, utilize physical reaction heat-dissipating, stirring 20 minutes is continued after making temperature rise to 170-180 DEG C, sulfuric acid and aniline is allowed fully to react, generate anilinesulfonic acid salt.After reaction terminates, anilinesulfonic acid salt is put into thermal oil tubular type through sulfonation reaction still bottom valve and bakes stove.
2, sulfonation, to bake: will the anilinesulfonic acid salt material in stove be baked, heated by heat-conducting oil pipes, control temperature is at 260 ± 3 DEG C, insulation 1h, make material generation translocation reaction, generate Sulphanilic Acid crude product, discharge a small amount of sulfur-bearing acid mist and aniline tail gas simultaneously, collected by collector and send into salify tail gas absorbing system.After translocation reaction terminates, take out material, through spontaneous combustion cooling, obtain the block crude product of Sulphanilic Acid canescence.Described translocation reaction is molecular transposition---refer to that a kind of quality of object and form are determined by molecule, the arrangement architecture of molecule changes, thus causes the change of mass of object form.
3, crude product is pulverized: by block for Sulphanilic Acid crude product, roll crusher be ground into 1-10 object particulate state with two roller, pulverize the tail gas of release simultaneously with dust collection trapping.
4, dissolving crude product: the Sulphanilic Acid crude product worm conveyor after pulverizing is closed in feeding dissolution kettle, add water and be mixed into solution, (part by weight of water and Sulphanilic Acid is 10:5.6), activated carbon is added again by the weight 0.8 ‰-3 ‰ of solution, pass through steam heating, maintain the temperature at 80-100 DEG C not stop to stir, Sulphanilic Acid fully dissolves, and is decoloured by charcoal absorption.
5, suction filtration: the Sulphanilic Acid solution dissolving decolouring is put into vacuumfilter suction filtration, makes the gac in solution and other impurity filtering, obtain purer Sulphanilic Acid solution.By the gac containing a small amount of waste residue after suction filtration, through high-temperature activation, make regenerated carbon.
6, crystallization, centrifugal: the filtrate after suction filtration is entered crystallization kettle, crystallization kettle circulating cooling water cooling, cooling temperature below 30 DEG C, crystallisation by cooling under constantly stirring, mixture after crystallisation by cooling puts into centrifuge dewatering, and the filter cake after dehydration is refining Sulphanilic Acid.The mother liquor that centrifuge dehydration goes out contains the Sulphanilic Acid of about 7%, and backspace solution still is for dissolving crude product.Mother liquor is after repeatedly reusing, and remaining impurity concentration increases and directly will have influence on quality product, needs to concentrate mother liquor, recrystallize, filtration, then filter cake is reverse back to dissolution kettle, and residue mother liquor is concentrated, produces still debris getting.Still debris getting is mainly the same molecule allosome works of Sulphanilic Acid and a small amount of vitriol concentrates water of condensation, then is recycled to dissolution kettle and recycles.
7, microwave drying: the moisture obtained containing 2.0% in Sulphanilic Acid is filtered in centrifuge dehydration, then enters microwave drying hopper, adopts microwave drying, control 3 minutes time of drying, dry to moisture < 0.5%, make product yield reach 99%, product purity reaches 99.5%.
8, weigh, pack, put in storage.
Claims (3)
1. a preparation method for Sulphanilic Acid solid phase method, is characterized in that: it comprises the following steps:
(1) salt-forming reaction: be first the sulfuric acid of 93% by levels, pump in high-order test tank with sulfuric acid pump, take 21.75 tons, sulfuric acid is added in sulfonation reaction still, with aniline pump, the aniline of levels 99% is pumped in the high-order test tank of aniline again, take 19.2 tons of aniline and sulfuric acid weight ratio is 1:1.1.33, open benzene peace test tank bottom valve, aniline is slowly dripped and adds in the sulfonation reaction still of sulfuric acid, after dripping, mixing and stirring, closed reactor, by steam heating, stirring 20 minutes is continued after making temperature rise to 170-180 DEG C, sulfuric acid and aniline is allowed fully to react, generate anilinesulfonic acid salt, after reaction terminates, anilinesulfonic acid salt is put into thermal oil tubular type through sulfonation reaction still bottom valve and bakes stove,
(2) sulfonation, to bake: will bake the anilinesulfonic acid salt material in stove, heated by heat-conducting oil pipes, control temperature is at 260 ± 3 DEG C, insulation 1h, make material generation translocation reaction, make molecular transposition, reaction generates Sulphanilic Acid crude product, discharge a small amount of sulfur-bearing acid mist and aniline tail gas simultaneously, collected by collector and send into salify tail gas absorbing system, after translocation reaction terminates, take out material, through spontaneous combustion cooling, obtain the block crude product of Sulphanilic Acid canescence;
(3) crude product is pulverized: by block for Sulphanilic Acid crude product, roll crusher be ground into 1-10 object particulate state with two roller, pulverize the tail gas of release simultaneously with dust collection trapping;
(4) dissolving crude product: the Sulphanilic Acid crude product worm conveyor after pulverizing is closed in feeding dissolution kettle, add water and be mixed into solution, the part by weight of water and Sulphanilic Acid is 10:5.6, activated carbon is added again by the weight 0.8 ‰-3 ‰ of solution, pass through steam heating, maintain the temperature at 80-100 DEG C not stop to stir, Sulphanilic Acid fully dissolves, and is decoloured by charcoal absorption;
(5) suction filtration: the Sulphanilic Acid solution dissolving decolouring is put into vacuumfilter suction filtration, makes the gac in solution and other impurity filtering, obtain purer Sulphanilic Acid solution;
(6) crystallization, centrifugal: the filtrate after suction filtration is entered crystallization kettle, crystallization kettle circulating cooling water cooling, cooling temperature below 30 DEG C, crystallisation by cooling under constantly stirring, mixture after crystallisation by cooling puts into centrifuge dewatering, and the filter cake after dehydration is refining Sulphanilic Acid;
(7) microwave drying: the moisture obtained containing 2.0% in Sulphanilic Acid is filtered in centrifuge dehydration, then enters microwave drying hopper, adopts microwave drying, control 3 minutes time of drying, dry to moisture < 0.5%, make product yield reach 99%, product purity reaches 99.5%;
(8) weigh, pack, put in storage.
2. the preparation method of Sulphanilic Acid solid phase method according to claim 1, is characterized in that: by the gac containing a small amount of waste residue after suction filtration, through high-temperature activation, make regenerated carbon.
3. the preparation method of Sulphanilic Acid solid phase method according to claim 1, it is characterized in that: the mother liquor that centrifuge dehydration goes out contains the Sulphanilic Acid of about 7%, backspace solution still is for dissolving crude product, mother liquor is after repeatedly reusing, remaining impurity concentration increases and directly will have influence on quality product, need to concentrate mother liquor, recrystallize, filter, again filter cake is reverse back to dissolution kettle, residue mother liquor, concentrated, produce still debris getting, still debris getting is mainly the same molecule allosome works of Sulphanilic Acid and a small amount of vitriol concentrates water of condensation, be recycled to dissolution kettle again to recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510462711.5A CN104974063A (en) | 2015-08-01 | 2015-08-01 | Preparation method of sulfanilic acid by solid-phase process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510462711.5A CN104974063A (en) | 2015-08-01 | 2015-08-01 | Preparation method of sulfanilic acid by solid-phase process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104974063A true CN104974063A (en) | 2015-10-14 |
Family
ID=54271080
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510462711.5A Pending CN104974063A (en) | 2015-08-01 | 2015-08-01 | Preparation method of sulfanilic acid by solid-phase process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104974063A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481735A (en) * | 2015-12-21 | 2016-04-13 | 沈阳化工研究院有限公司 | Method for preparing aniline-2-sulfonic acid |
| CN107522336A (en) * | 2017-09-08 | 2017-12-29 | 江苏明盛化工有限公司 | The processing method of caused acid waste water in a kind of contraposition ester production process |
| CN109323590A (en) * | 2018-10-30 | 2019-02-12 | 阜阳市四通化工有限公司 | A kind of p-aminobenzene sulfonic acid solidifies the preparation method of indexable furnace and p-aminobenzene sulfonic acid |
| CN113121392A (en) * | 2019-12-30 | 2021-07-16 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN116715607A (en) * | 2023-06-08 | 2023-09-08 | 浙江宏达化学制品有限公司 | Method for synthesizing sulfanilic acid |
-
2015
- 2015-08-01 CN CN201510462711.5A patent/CN104974063A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 徐伟民 等: "《基础化学实验》", 31 July 2011, 浙江大学出版社 * |
| 王鸿 等: "用浓硫酸磺化苯胺制备对氨基苯磺酸生产工艺浅析", 《湖北化工》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481735A (en) * | 2015-12-21 | 2016-04-13 | 沈阳化工研究院有限公司 | Method for preparing aniline-2-sulfonic acid |
| CN107522336A (en) * | 2017-09-08 | 2017-12-29 | 江苏明盛化工有限公司 | The processing method of caused acid waste water in a kind of contraposition ester production process |
| CN109323590A (en) * | 2018-10-30 | 2019-02-12 | 阜阳市四通化工有限公司 | A kind of p-aminobenzene sulfonic acid solidifies the preparation method of indexable furnace and p-aminobenzene sulfonic acid |
| CN113121392A (en) * | 2019-12-30 | 2021-07-16 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN113121392B (en) * | 2019-12-30 | 2022-06-10 | 上海合丽亚化工科技有限公司 | Aminobenzene sulfonic acid compound crystal particles and preparation method thereof |
| CN116715607A (en) * | 2023-06-08 | 2023-09-08 | 浙江宏达化学制品有限公司 | Method for synthesizing sulfanilic acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104974063A (en) | Preparation method of sulfanilic acid by solid-phase process | |
| CN101693701B (en) | Purification process for vulcanization accelerator 2-mercaptobenzothiazole | |
| CN103146221B (en) | Method and device for continuously producing dyes | |
| CN104003427B (en) | A kind of preparation method with spodumene Concentrate sheet Lithium hydroxide | |
| CN105967415B (en) | A kind of beta naphthal high-concentration organic substance wastewater process for reclaiming with high salt and system | |
| CN104016893A (en) | A preparing method of 4,4'-sulfonyldiphenol | |
| CN105017028B (en) | The improvement synthetic method of o-phenylenediamine is prepared in a kind of ortho-nitraniline reduction | |
| CN106083660A (en) | A kind of preparation technology of 1 amino 4 bromo anthraquinone 2 sodium sulfonate | |
| CN103964600B (en) | A kind of recoverying and utilizing method of azo dispersion dyes waste water | |
| CN101219977A (en) | CLT acid production method without acid waste liquid discharge | |
| CN102320635A (en) | Comprehensive utilization method of waste sulfuric acid of sulfonated products | |
| CN107522336A (en) | The processing method of caused acid waste water in a kind of contraposition ester production process | |
| CN101817791B (en) | Method for directly producing water soluble aniline black | |
| CN101759570B (en) | Preparation method of p-nitrophenol | |
| CN109971200A (en) | A kind of recycling preparation method of disperse orange dye | |
| CN107473943A (en) | A kind of preparation method of 2,6 orcin | |
| CN105110537B (en) | A kind for the treatment of of DSD acid oxidized waste water and its recovery method as resource | |
| CN102336690B (en) | Method for separating and purifying high-purity 4,4'-dihydroxydiphenylsulfone | |
| CN102391163A (en) | Preparation method of sulfonated para-ester serving as dye intermediate | |
| CN104725282A (en) | Novel environment-friendly production process of 1-naphthol-4-sulfonic acid | |
| CN105524485B (en) | A kind of preparation method of active red dye | |
| CN104610173B (en) | A kind of cycle production process of nigrosine | |
| CN107986998A (en) | A kind of process for cleanly preparing of sulfonated para-ester serving as dye intermediate | |
| CN105440737B (en) | A kind of preparation method of energy saving and environment friendly disperse dyes | |
| CN208545340U (en) | A kind of device preparing phthalimide using phthalic anhydride heavy constituent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20151014 |
|
| RJ01 | Rejection of invention patent application after publication |