CN105859581A - New nitration technology used in production of 2-cyano-4-nitro chlorobenzene - Google Patents
New nitration technology used in production of 2-cyano-4-nitro chlorobenzene Download PDFInfo
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- CN105859581A CN105859581A CN201610250600.2A CN201610250600A CN105859581A CN 105859581 A CN105859581 A CN 105859581A CN 201610250600 A CN201610250600 A CN 201610250600A CN 105859581 A CN105859581 A CN 105859581A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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Abstract
The invention belongs to the field of chemical industry, and relates to a new nitration technology used in production of 2-cyano-4-nitro chlorobenzene. The new nitration technology takes o-chlorobenzonitrile as a raw material and uses mixed acid prepared from medium-concentration sulfuric acid and medium-concentration nitric acid as a solvent, and comprises the steps of dissolving the o-chlorobenzonitrile by using the solvent, and carrying out a nitration reaction at the medium temperature. The new nitration technology completely overcomes the defects that in the traditional technology, the electric energy consumption is high since high-concentration sulfuric acid and high-concentration nitric acid are used for carrying out the nitration reaction at low temperature, and the quality of the 2-cyano-4-nitro chlorobenzene is reduced if the temperature is slightly high.
Description
Technical field
The present invention relates to process for nitrification during a kind of 2-cyano group-4-nitro chlorobenzene produces.
Background technology
During 2-cyano group-4-nitro chlorobenzene produces, traditional nitration processes is with o-chloro benzonitrileFor raw material, utilize the concentrated sulphuric acid of about 98% to do solvent acid and dissolve o-chloro benzonitrile, with 98%
The concentrated sulphuric acid of left and right and the concentrated nitric acid of about 98% are made into mixed acid at about 0-10 DEG C low temperature nitrification, generation 2-
Cyano group-4-nitro chlorobenzene.This technique is tight to the concentration requirement of sulphuric acid and nitric acid, as slightly lower in concentration can affect 2-
Cyano group-4-nitro chlorobenzene quality.Nitration reaction requires to carry out at low temperatures, it is necessary to lower the temperature with chilled brine,
Consuming substantial amounts of electric energy, temperature is slightly higher, and 2-cyano group-4-nitro chlorobenzene quality will reduce.
Summary of the invention
The goal of the invention of the present invention is that nitrification in offer a kind of 2-cyano group-4-nitro chlorobenzene production
New technology, is characterized in that making solvent acid with the nitric acid preparation nitration mixture of the sulphuric acid of intermediate concentration with intermediate concentration dissolves
O-chloro benzonitrile, carries out nitration reaction at moderate temperatures, overcomes traditional use high-concentration sulfuric acid, nitric acid completely
The shortcoming of nitrification at low temperatures.
The technical scheme is that process for nitrification in the production of 2-cyano group-4-nitro chlorobenzene, its
Step is as follows:
1) measured 564 kilograms of o-chloro benzonitriles by o-chloro benzonitrile measuring tank and add nitrating pot；
2) being respectively configured mass concentration in measuring tank is 75%-95% and mass concentration is that 80%-95% nitric acid is molten
Liquid, during configuration, temperature is located at 11 DEG C-60 DEG C；Measure 1500-1900kg sulfuric acid solution and 220-300kg respectively
Salpeter solution, is slowly added in nitration mixture preparation still；Add nitration mixture measuring tank after mix homogeneously, measure 500-600kg
Mixed acid solution, mixed acid solution is added in nitration reaction still；
3) in 11 DEG C of-60 DEG C of moderate temperatures, carry out nitration reaction, react 2-4 hour, generate 2-cyanogen
Base-4-nitro chlorobenzene.
Described raw-material inventory and quality standard such as table 1
Table 1 raw material inventory and quality standard
Table 1
The invention have the benefit that
1, the present invention uses the nitric acid preparation nitration mixture with the sulphuric acid of intermediate concentration with intermediate concentration, relative to concentration
Being sulphuric acid, the nitric acid of 98% of 98%, the cost of raw material is substantially reduced.
2, the temperature range of its nitration reaction is interval wide, it is easy to controls, and can be cooled with circulating water cooling,
Need not use chilled brine, saved the energy.Chilled brine 50 tons, joint is saved according to every batch, statistical data
About electric energy 344 kilowatt hour.According to producing at present 4000 batches of calculating per year, year saves energy 1376 megawatt hour.
Following table is saves energy statistical table:
| Lot number | 1 | 4000 |
| Saves energy/kilowatt hour | 344 | 1376000 |
3, the 2-cyano group-4-nitro chlorobenzene product quality that the present invention is produced is high: with the sulphuric acid of intermediate concentration
Prepare nitration mixture with the nitric acid of intermediate concentration, carry out nitration reaction at moderate temperatures, 2-cyano group-4-in product
2-cyano group-4-the nitro chlorobenzene that nitro chlorobenzene content obtains higher than the low temperature nitration reaction of high concentration nitration mixture
Content.
Following table is different nitrification mode Product checking Comparative result tables:
| Nitrification mode | 2-cyano group-4-nitro chlorobenzene % | Six nitre % | Benzene eyeball % |
| Middle temperature nitrification | 97.65 | 1.56 | 0.11 |
| Low temperature nitrification | 97.22 | 1.98 | 0.05 |
Accompanying drawing explanation
Fig. 1 is the process chart of the embodiment of the present invention.
Detailed description of the invention
Embodiment 1
One embodiment of the invention, by the sulfuric acid solution of intermediate concentration and the salpeter solution of intermediate concentration at measuring tank
In weigh appropriate amount be slowly added to nitration mixture preparation still, after mix homogeneously add nitration mixture measuring tank, weigh appropriate amount
Nitration reaction still is added by nitration mixture measuring tank；By measuring tank weighing the o-chloro benzonitrile of 654kg by o-chloro benzonitrile
Add nitration reaction still；Carrying out nitration reaction in 11 DEG C of-60 DEG C of moderate temperatures, nitration mixture stirs after adding
1 hour sampling detection product content.Its process can be as shown in Figure 1.
Above-mentioned raw material inventory and quality standard are as shown in table 2 below, are by the sulphuric acid 1600kg that concentration is 90%
Nitration mixture processed, nitration mixture consumption 693kg, the adjacent chlorobenzene of concentration >=99% is mixed with the nitric acid 305kg that concentration is 90%
Nitrile consumption 564kg.
Product content is as shown in table 3, and 2-cyano group-4-nitro chlorobenzene content 97.95%, six nitre content 1.28%/,
Cyanophenyl content 0.17%.
Table 2 raw material inventory and quality standard
Table 2
Table 3 product content table
Table 3
| Purity % | Six nitre % | Cyanophenyl % |
| 97.95 | 1.28 | 0.17 |
Embodiment 2
One embodiment of the invention, by the sulfuric acid solution of intermediate concentration and the salpeter solution of intermediate concentration at measuring tank
In weigh appropriate amount be slowly added to nitration mixture preparation still, after mix homogeneously add nitration mixture measuring tank, weigh appropriate amount
Nitration reaction still is added by nitration mixture measuring tank；By measuring tank weighs appropriate o-chloro benzonitrile, o-chloro benzonitrile is added
Nitration reaction still；Carrying out nitration reaction in 11 DEG C of-60 DEG C of moderate temperatures, it is little that nitration mixture stirs 1 after adding
Time sampling detection product content.Its process can be as shown in Figure 1.
Raw-material specification and inventory are as shown in table 4 below, are the sulphuric acid 1800kg by concentration 80% and concentration
The nitric acid 340kg of 85% mixes nitration mixture processed, nitration mixture consumption 850kg, the o-chloro benzonitrile consumption of concentration >=99%
564kg。
Product content such as table 5 shows, 2-cyano group-4-nitro chlorobenzene content 97.14%, six nitre content 1.98%,
Cyanophenyl content 0.13%.
Table 4 specifications of raw materials and the scale that feeds intake
Table 4
Table 5 product content table
Table 5
| Purity % | Six nitre % | Benzene eyeball % |
| 97.14 | 1.98 | 0.13 |
Claims (1)
- Process for nitrification in the production of 1.2-cyano group-4-nitro chlorobenzene, it is characterised in that the step of this technique is such as Under:A) measured 564 kilograms of o-chloro benzonitriles by o-chloro benzonitrile measuring tank and add nitration reaction still；B) being respectively configured mass concentration in measuring tank is 75%-95% and mass concentration is that 80%-95% nitric acid is molten Liquid, during configuration, temperature is located at 11 DEG C-60 DEG C；Measure 1500-1900kg sulfuric acid solution and 220-300kg respectively Salpeter solution, is slowly added in nitration mixture preparation still；Add nitration mixture measuring tank after mix homogeneously, measure 500-600kg Mixed acid solution, mixed acid solution is added in nitration reaction still；C) in 11 DEG C of-60 DEG C of moderate temperatures, carry out nitration reaction, react 2-4h, generate 2-cyano group-4- Nitro chlorobenzene.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610250600.2A CN105859581A (en) | 2016-04-21 | 2016-04-21 | New nitration technology used in production of 2-cyano-4-nitro chlorobenzene |
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| CN201610250600.2A CN105859581A (en) | 2016-04-21 | 2016-04-21 | New nitration technology used in production of 2-cyano-4-nitro chlorobenzene |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369453A (en) * | 2018-09-04 | 2019-02-22 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 5- nitrobenzonitrile of 2- |
| CN110041228A (en) * | 2019-05-15 | 2019-07-23 | 浙江长华科技股份有限公司 | A kind of o-chloro benzonitrile nitration processes |
| CN110128295A (en) * | 2019-05-16 | 2019-08-16 | 浙江长华科技股份有限公司 | A kind of production technology based on micro- reaction synthesis chloro- 5- nitrobenzonitrile of 2- |
| CN113480449A (en) * | 2021-07-05 | 2021-10-08 | 河北嘉泰化工科技有限公司 | Novel process for continuously nitrifying and synthesizing 2-cyano-4-nitrochlorobenzene by solvent method |
| CN114634422A (en) * | 2022-03-14 | 2022-06-17 | 河北中科金辉药业有限公司 | Preparation method of dinitolmide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203905A (en) * | 1998-07-14 | 1999-01-06 | 辽河油田金海化工厂 | New process for synthetising m-nitrobenzoic |
| CN105418458A (en) * | 2015-12-18 | 2016-03-23 | 孝感华越机电科技有限公司 | Synthetic process of 2-cyano-4-nitroaniline |
-
2016
- 2016-04-21 CN CN201610250600.2A patent/CN105859581A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203905A (en) * | 1998-07-14 | 1999-01-06 | 辽河油田金海化工厂 | New process for synthetising m-nitrobenzoic |
| CN105418458A (en) * | 2015-12-18 | 2016-03-23 | 孝感华越机电科技有限公司 | Synthetic process of 2-cyano-4-nitroaniline |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369453A (en) * | 2018-09-04 | 2019-02-22 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 5- nitrobenzonitrile of 2- |
| CN109369453B (en) * | 2018-09-04 | 2021-06-25 | 浙江工业大学 | Method and device for preparing 2-chloro-5-nitrobenzonitrile through pipelining |
| CN110041228A (en) * | 2019-05-15 | 2019-07-23 | 浙江长华科技股份有限公司 | A kind of o-chloro benzonitrile nitration processes |
| CN110128295A (en) * | 2019-05-16 | 2019-08-16 | 浙江长华科技股份有限公司 | A kind of production technology based on micro- reaction synthesis chloro- 5- nitrobenzonitrile of 2- |
| CN113480449A (en) * | 2021-07-05 | 2021-10-08 | 河北嘉泰化工科技有限公司 | Novel process for continuously nitrifying and synthesizing 2-cyano-4-nitrochlorobenzene by solvent method |
| CN114634422A (en) * | 2022-03-14 | 2022-06-17 | 河北中科金辉药业有限公司 | Preparation method of dinitolmide |
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