CN106083664A - A kind of nitro compounds method of reducing - Google Patents
A kind of nitro compounds method of reducing Download PDFInfo
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- CN106083664A CN106083664A CN201610399081.6A CN201610399081A CN106083664A CN 106083664 A CN106083664 A CN 106083664A CN 201610399081 A CN201610399081 A CN 201610399081A CN 106083664 A CN106083664 A CN 106083664A
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- Prior art keywords
- nitro compounds
- reducing
- acid
- technique
- percentage
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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
- C07C303/22—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 from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
Abstract
A kind of nitro compounds method of reducing, the percentage by weight of its component is: nitro compounds (2 nitronaphthalenes 4,8, disulfonic acid) 5% 20%, reducing agent (industrial sodium sulfide) 3% 30%, water 50% 90%, 98% sulphuric acid 5% 15%, the percentage by weight sum of each component is 100%.Reaction temperature 20 100 DEG C.1 12 hours response time；Nitro compounds (2 nitronaphthalene 4,8 disulfonic acid) can be reduced by this technique, obtain amino substance (2 naphthylamines 4,8 disulfonic acid).Reaction condition is gentleer, and course of reaction is easily controlled；Alternate country eliminates technique iron powder reducing technique；Do not produce hazardous waste reduction iron cement；Production process produces side-product sulfur can utilize；The product quality produced is as iron powder reducing technique；The yield of product is slightly above iron powder reducing technique.
Description
Technical field
The present invention relates to a kind of nitro compounds (2-nitronaphthalene-4,8-disulfonic acid) reducing process and amino substance thereof (2-naphthylamines-4,
8-disulfonic acid) preparation method, belong to fine chemistry industry class.
Background technology
Currently available technology, produces 2-naphthylamines-4,8-disulfonic acid commonly used iron powder reducing technique the most both at home and abroad.This work
Skill has been listed country in and has been eliminated technique.
Summary of the invention
It is an object of the invention to: providing a kind of nitro compounds method of reducing, it has the feature without waste gas and discharge of wastewater, nothing
Polluting, purity is high.
The present invention is achieved in that a kind of nitro compounds method of reducing, and the percentage by weight of its component is:
Nitro compounds 5%-20%；Industrial sodium sulfide 3%-30%；
Water 50%-85%；98% sulphuric acid 5%-15%；
The percentage by weight sum of each component is 100%；
Reaction temperature 20-100 DEG C；
1-15 hour response time.
Described a kind of nitro compounds method of reducing, it is characterized in that described nitro compounds is 2-nitronaphthalene-4,8 ,-two sulphurs
Acid.
Described a kind of nitro compounds method of reducing, it is characterized in that described industry akali sulphide is for industry alkalization sodium.
Described a kind of nitro compounds method of reducing, comprises the steps:
Water, industry akali sulphide, nitro compounds being put in reactor, opens stirring, be warming up to 20 100 DEG C simultaneously, insulation is anti-
Answering 1 15 hours, be subsequently adding 60% to the highly acid of sulphuric acid total amount, pH value is 1-2, filters and sloughs sulfur, is concentrated into amino substance
Content 10 30%, adds residual sulfuric acid, can separate out amino substance, filters, and dries, obtains amino substance, be packaged as finished product.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 15%,
Industrial sodium sulfide 12%,
Water 65%,
Sulphuric acid 8%,
Reaction temperature 45 DEG C.
12 hours response time.
Reducing process and amino substance preparation method:
Water, industry akali sulphide, nitro compounds (2-nitronaphthalene-4,8-disulfonic acid) are put in reactor, opens stirring, simultaneously
It is warming up to 45 DEG C, insulation reaction 12 hours, it is subsequently adding sulphuric acid to highly acid, pH is 1-2, filters and sloughs sulfur, is concentrated into ammonia
Substrates content about 18%, adds residual sulfuric acid, can separate out amino substance, filters, and dries, obtains amino substance, be packaged as finished product.
The advantage of this technique is: reaction condition is gentleer, and course of reaction is easily controlled；Alternate country eliminates technique ferrum
Powder reducing process；Do not produce hazardous waste reduction iron cement；Production process produces side-product sulfur can utilize；The product produced
Quality is as iron powder reducing technique；The yield of product is slightly above iron powder reducing technique.
Embodiment 2
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 18%
Industrial sodium sulfide 16%
Water 56%
Sulphuric acid 10%
Reaction temperature 85 DEG C.
4 hours response time.
Embodiment 3
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 10%
Industrial sodium sulfide 14%
Water 69%
Sulphuric acid 7%
Reaction temperature 80 DEG C.
5 hours response time.
Embodiment 4
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 6%
Industrial sodium sulfide 6%
Water 82%
Sulphuric acid 6
Reaction temperature 80 DEG C.
6 hours response time.
Embodiment 5
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 13%
Industrial sodium sulfide 14%
Water 65%
Sulphuric acid 8%
Reaction temperature 50 DEG C.
14 hours response time.
Embodiment 6
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 15%
Industrial sodium sulfide 14%
Water 61%
Sulphuric acid 10%
Reaction temperature 90 DEG C.
8 hours response time.
Embodiment 7
A kind of nitro compounds method of reducing, the percentage by weight of its component is:
Nitro compounds (2-nitronaphthalene-4,8 ,-disulfonic acid) 25%
Industrial sodium sulfide 18%
Water 50%
Sulphuric acid 7%
Reaction temperature 80 DEG C.
11 hours response time.
Above-described is only the preferred embodiments of the present invention.It should be pointed out that, for the ordinary skill of this area
For personnel, without departing from the principles of the present invention, it is also possible to make some improvement and modification, this is also considered as the present invention's
Protection domain.
Claims (5)
1. a nitro compounds method of reducing, it is characterised in that: the percentage by weight of its component is:
Nitro compounds 5%-20%, industrial sodium sulfide 3%-30%, water 50%-85%, 98% sulphuric acid 5%-15%,
The percentage by weight sum of each component is 100%；
Reaction temperature 20-100 DEG C；
1-15 hour response time.
A kind of nitro compounds method of reducing, it is characterised in that: described nitro compounds is 2-nitronaphthalene-4,
8 ,-disulfonic acid.
A kind of nitro compounds method of reducing, it is characterised in that: described industry akali sulphide is industry alkalization
Sodium.
A kind of nitro compounds method of reducing, it is characterised in that: described 98% sulphuric acid is industrial dense sulfur
Acid.
A kind of nitro compounds method of reducing, it is characterised in that: described reducing process and amino substance system thereof
Preparation Method comprises the steps:
Water, industry akali sulphide, nitro compounds are put in reactor, opens stirring, be warming up to 20-100 DEG C, insulation reaction 1-simultaneously
15 hours, being subsequently adding 60% to the highly acid of sulphuric acid total amount, pH value is 1-2, filters and sloughs sulfur, is concentrated into amino substance content
10-30%, adds residual sulfuric acid, can separate out amino substance, filters, and dries, obtains amino substance, be packaged as finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610399081.6A CN106083664A (en) | 2016-06-06 | 2016-06-06 | A kind of nitro compounds method of reducing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610399081.6A CN106083664A (en) | 2016-06-06 | 2016-06-06 | A kind of nitro compounds method of reducing |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106083664A true CN106083664A (en) | 2016-11-09 |
Family
ID=57227403
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610399081.6A Pending CN106083664A (en) | 2016-06-06 | 2016-06-06 | A kind of nitro compounds method of reducing |
Country Status (1)
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| CN (1) | CN106083664A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437111A (en) * | 2019-08-26 | 2019-11-12 | 辽宁大学 | A method of synthesis C acid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3700605A (en) * | 1969-04-18 | 1972-10-24 | Ici Ltd | Catalysts |
| CN1260346A (en) * | 1998-12-01 | 2000-07-19 | 拜尔公司 | Method for preparing amino-aryl sulfonic acid |
| RU2159424C2 (en) * | 1998-12-23 | 2000-11-20 | Государственный научный центр Российской Федерации "НИОПИК" | Procedure determining aromatic nitrocompounds and products for their reduction |
| CN101301608A (en) * | 2008-06-26 | 2008-11-12 | 南京大学 | Silicon dioxide supported nano-silver catalyst, preparation and use thereof |
| CN102911510A (en) * | 2012-10-25 | 2013-02-06 | 上海贝通色彩科技有限公司 | Ink-jet dye compound and preparation method thereof |
| CN105017028A (en) * | 2015-07-27 | 2015-11-04 | 江阴市华亚化工有限公司 | Improved synthetic method for preparing o-phenylenediamine by reducing o-nitroaniline |
| CN105481728A (en) * | 2015-12-25 | 2016-04-13 | 铜陵化工集团有机化工有限责任公司 | Preparation method of 1-naphthylamino-8-sulfonic acid |
-
2016
- 2016-06-06 CN CN201610399081.6A patent/CN106083664A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3700605A (en) * | 1969-04-18 | 1972-10-24 | Ici Ltd | Catalysts |
| CN1260346A (en) * | 1998-12-01 | 2000-07-19 | 拜尔公司 | Method for preparing amino-aryl sulfonic acid |
| RU2159424C2 (en) * | 1998-12-23 | 2000-11-20 | Государственный научный центр Российской Федерации "НИОПИК" | Procedure determining aromatic nitrocompounds and products for their reduction |
| CN101301608A (en) * | 2008-06-26 | 2008-11-12 | 南京大学 | Silicon dioxide supported nano-silver catalyst, preparation and use thereof |
| CN102911510A (en) * | 2012-10-25 | 2013-02-06 | 上海贝通色彩科技有限公司 | Ink-jet dye compound and preparation method thereof |
| CN105017028A (en) * | 2015-07-27 | 2015-11-04 | 江阴市华亚化工有限公司 | Improved synthetic method for preparing o-phenylenediamine by reducing o-nitroaniline |
| CN105481728A (en) * | 2015-12-25 | 2016-04-13 | 铜陵化工集团有机化工有限责任公司 | Preparation method of 1-naphthylamino-8-sulfonic acid |
Non-Patent Citations (2)
| Title |
|---|
| 刘效标: "以硫化钠直接还原苦味酸", 《爆破器材》 * |
| 王红英等: "硫化钠还原制备邻氨基苯甲酸的研究", 《安徽化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110437111A (en) * | 2019-08-26 | 2019-11-12 | 辽宁大学 | A method of synthesis C acid |
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Application publication date: 20161109 |
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