CN106278908A - Large red-based g production new technique - Google Patents
Large red-based g production new technique Download PDFInfo
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- CN106278908A CN106278908A CN201510245336.9A CN201510245336A CN106278908A CN 106278908 A CN106278908 A CN 106278908A CN 201510245336 A CN201510245336 A CN 201510245336A CN 106278908 A CN106278908 A CN 106278908A
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Abstract
The present invention relates to a kind of large red-based g production new technique, large red-based g belongs to the important composition thing of azoic dyes insoluble azo dyes, it is mainly used in dyeing and the stamp of bafta, large red (i.e. flag is red) is contaminated with azoic coupling component AS or AS-D coupling, can also be used for the dyeing of silk, viscose glue and nylon fabric, also serve as the intermediate of organic pigment.The present invention use nitric acid to mix by 1:1.3 with sulphuric acid in nitrifying process after nitrification, 50% sulphuric acid recycle the mobility of the system of improve, conductivity, use liquefied ammonia to be neutralized and obtain the side-product that added value is of a relatively high, the nitrification stage expands kettle and amasss, and material is 316L, while chuck is lowered the temperature, in still, add 5 built-in coil pipes, substantially increase rate of temperature fall.The present invention have pollution-free, the high and low energy consumption of yield, by-product recycle, by-product added value advantages of higher, economic benefit of the present invention and environmental benefit are high.
Description
Technical field
The present invention relates to the production new technique of a kind of large red-based g, the new synthesis process of specific design to fine chemical product water dyestuff (2 amino 4 Methylnitrobenzene).
Background technology
Water dyestuff large red-based g, formal name used at school 2-amino-4-Methylnitrobenzene, belong to the important composition thing of azoic dyes insoluble azo dyes, be mainly used in dyeing and the stamp of bafta..Product content is more than 98%, fusing point 107 DEG C.Large red-based g is golden yellow crystal.Water insoluble, it is dissolved in ethanol, ether, benzene and acetone.Coupling ability is strong, and coupling speed is medium.It is mainly used in dyeing and the stamp of bafta, contaminates large red (i.e. flag is red) it can also be used to the dyeing of silk, viscose glue and nylon fabric with azoic coupling component AS or AS-D coupling, also serve as the intermediate of organic pigment.
At present, existing large red-based g production technology is to use ortho-aminotoluene nitrification after 98% sulphuric acid becomes salt, then neutralization obtains.Concrete technology flow process, for adding 98% sulphuric acid in a kettle., is slowly added dropwise ortho-aminotoluene at about 25 DEG C, then is slowly added dropwise nitric acid and carries out nitrification.Course of reaction to guarantee in the case of ortho-aminotoluene is completely dissolved, and temperature controls to drip nitric acid between 5 DEG C 0 DEG C.Carrying out elutriation after dropping below 60 DEG C, treat that temperature is down to less than 35 DEG C and is started centrifugal to obtain solid, solid adds after 20% sodium carbonate liquor neutralizes centrifugal after dissolving, and is centrifuged out solid and obtains product large red-based g exactly.But currently used large red-based g production technology also exists problems, (1) simple nitric acid carries out nitrification, and to be belonging to a dangerization reaction, therefore potential safety hazard big, and energy consumption is high.(2) neutralizing post uses 20% sodium carbonate can produce low value-added waste water, processes more difficult, to environmentally undesirable.(3) centrifugal after elutriation to obtain a large amount of 50% dilute sulfuric acid economic worth the highest, it is impossible to recycles, does not meets atom economy type requirement.Owing to there are above-mentioned problems, existing large red-based g production technology is badly in need of improving.
Summary of the invention
In order to solve the deficiency on above-mentioned existing technology and equipment, the present invention provides a kind of large red-based g production new technique.
The concrete technology flow process of the present invention is:
Workshop section one: become salt nitrification
(1) in 1000L stainless steel cauldron, 98% concentrated sulphuric acid 800Kg is pumped into, 50% sulphuric acid 200Kg；
(2) control temperature is between 20 DEG C 25 DEG C, is slowly added to ortho-aminotoluene 220kg, and time for adding controls at 2 hours, is incubated after completion of dropwise addition；
(3) insulation 2 hours, are completely dissolved into salt to ortho-aminotoluene, open chilled brine and prepare cooling；
(4) being down to 5 DEG C of preparations when temperature and be slowly added dropwise nitration mixture (98% sulphuric acid and 98% nitric acid are mixed by 1:1.3) 230Kg, time for adding controls, at 7 hours, to drip complete preparation elutriation；
(5) adding 700Kg tap water in advance in 2000L elutriation still, nitrification material is slowly put into elutriation still, nitrification material dissolubility in 50% sulfuric acid solution is minimum, will separate out with crystal completely, prepares centrifugal after being cooled to room temperature；
(6) obtain solid after machine is centrifugal by centrifugation and become salt itrated compound material and 50% sulfuric acid solution.
Workshop section two: neutralize
(1) putting into nitrification material 1300Kg after adding tap water 2t in 5000L reactor and be warming up to 80 DEG C, insulation, to being completely dissolved, is stirred；
(2) control temperature is at about 55 DEG C, is slowly introducing liquefied ammonia, and regulation PH is to neutral, and golden yellow crystal constantly separates out；
(3) starting to be centrifuged after being cooled to room temperature, obtain golden yellow crystal and be finished product, the ammonium sulfate in mother solution reclaims for agricultural production.
Compared with conventional art, the invention has the beneficial effects as follows that (1) has carried out reformed AHP, side-product 50% sulphuric acid and 98% sulphuric acid and has been used in mixed way original technique, the cost of material not only reduced, also mobility, the conductivity of whole response system is substantially improved.(2) nitrifying process is the most simply carried out with 98% nitric acid, but carry out nitrification with the nitration mixture (1:1.4) of 98% nitric acid and 98% sulphuric acid, not only reduce the danger coefficient of nitrifying process, and improve the low temperature environment required for reaction, greatly reducing energy consumption, product yield is brought up to 88% by traditional handicraft 73%.(3) neutralizing workshop section is not using 20% sodium carbonate to be adjusted PH, but uses liquefied ammonia, has obtained the byproduct of ammonium sulfate that added value is high.(4) nitrification workshop section uses 1000L stainless steel cauldron, and material is 316L, and at chuck the most built-in 5 coil pipes of cooling, substantially increases rate of temperature fall.
Accompanying drawing explanation
Fig. 1 is large red-based g production new technique technological process of the present invention.
Detailed description of the invention
The present invention is further described below in conjunction with the accompanying drawings.
98% concentrated sulphuric acid 800Kg, 50% sulphuric acid 200Kg is pumped in 1000L reactor；Control temperature, between 20 DEG C 25 DEG C, is slowly added to ortho-aminotoluene 220kg, and time for adding controls at 2 hours, is incubated after completion of dropwise addition；It is incubated 2 hours, is completely dissolved into salt to ortho-aminotoluene, open chilled brine and prepare cooling；Being down to 5 DEG C of preparations when temperature and be slowly added dropwise nitration mixture (98% sulphuric acid and 98% nitric acid are mixed by 1:1.3) 230Kg, time for adding controls, at 7 hours, to drip complete preparation elutriation；Adding 700Kg tap water in advance in 2000L elutriation still, nitrification material is slowly put into elutriation still, nitrification material dissolubility in 50% sulfuric acid solution is minimum, will separate out with crystal completely, prepares centrifugal after being cooled to room temperature；Obtain solid after machine is centrifugal by centrifugation and become salt itrated compound material and 50% sulfuric acid solution.Putting into nitrification material 1300Kg after adding tap water 2t in 5000L reactor and be warming up to 80 DEG C, insulation, to being completely dissolved, is stirred；Control temperature, at about 55 DEG C, is slowly introducing liquefied ammonia, and regulation PH is to neutral, and golden yellow crystal constantly separates out；Starting to be centrifuged after being cooled to room temperature, obtain golden yellow crystal and be finished product, the ammonium sulfate in mother solution reclaims for agricultural production, product inspection qualified packaging warehouse-in.
Claims (6)
1. a large red-based g production new technique, it is characterised in that: described technological process includes:
Workshop section one: become salt nitrification
98% sulphuric acid and part 50% sulphuric acid is added, stirring in reactor；
It is slowly added dropwise ortho-aminotoluene, is incubated after completion of dropwise addition to becoming salt；
Insulation terminates, and is slowly added dropwise nitration mixture and carries out nitrification；
Workshop section two: neutralize
Adding water and elutriation material in reactor, stirring is to dissolving；
After dissolving completely, cooling, is neutralized to neutrality；
Continue cooling, be centrifugally separating to obtain product.
2. large red-based g production new technique as claimed in claim 1, it is characterised in that: becoming sal prunella chemical industry section 98% sulphuric acid 800Kg, 50% sulphuric acid 200Kg, the two feeds intake according to mass ratio 1:4.
3. large red-based g production new technique as claimed in claim 1, it is characterised in that: becoming sal prunella chemical industry section to be slowly added dropwise ortho-aminotoluene and control temperature between 20 DEG C 25 DEG C, time for adding is about 2 hours, and temperature retention time is half an hour.
4. large red-based g production new technique as claimed in claim 1, it is characterised in that: becoming the nitration mixture utilized in sal prunella chemical industry section is to carry out nitrification according to 98% sulphuric acid and 98% nitric acid mass ratio 1:1.3 between 5 DEG C 0 DEG C.
5. red base G production new technique as claimed in claim 1, it is characterised in that: neutralizing workshop section's solution temperature is 80 DEG C, and dissolving amount of water is 5 times of end product quality.
6. red base G production new technique as claimed in claim 1, it is characterised in that: neutralizing workshop section's regulation pH value and use liquefied ammonia, the temperature continuing to be cooled to separate out completely have to be lower than 35 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510245336.9A CN106278908A (en) | 2015-05-15 | 2015-05-15 | Large red-based g production new technique |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510245336.9A CN106278908A (en) | 2015-05-15 | 2015-05-15 | Large red-based g production new technique |
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| CN106278908A true CN106278908A (en) | 2017-01-04 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851127A (en) * | 2019-02-01 | 2019-06-07 | 山东世纪阳光科技有限公司 | A kind of processing method of large red-based g spent acid |
| CN109942434A (en) * | 2019-03-26 | 2019-06-28 | 山东世纪阳光科技有限公司 | A kind of production method of large red-based g |
| CN113121360A (en) * | 2019-12-30 | 2021-07-16 | 青岛海湾精细化工有限公司 | Preparation method of scarlet base G |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045592A (en) * | 1989-03-13 | 1990-09-26 | 镇江市染料化工二厂 | A kind of production method of glacial dye |
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2015
- 2015-05-15 CN CN201510245336.9A patent/CN106278908A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045592A (en) * | 1989-03-13 | 1990-09-26 | 镇江市染料化工二厂 | A kind of production method of glacial dye |
Non-Patent Citations (4)
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| SHENG CHANG等: "Design and Synthesis of Novel 2-Phenylaminopyrimidine (PAP)Derivatives and Their Antiproliferative Effects in HumanChronic Myeloid Leukemia Cells", 《MOLECULES》 * |
| 单居正，陈远静: "我国工业废硫酸的处理情况", 《化工环保》 * |
| 叶思景 等: "5-氨基邻甲苯酚的合成工艺研究", 《广东化工》 * |
| 黄信德 等: "大红色基G的合成", 《宁波化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851127A (en) * | 2019-02-01 | 2019-06-07 | 山东世纪阳光科技有限公司 | A kind of processing method of large red-based g spent acid |
| CN109942434A (en) * | 2019-03-26 | 2019-06-28 | 山东世纪阳光科技有限公司 | A kind of production method of large red-based g |
| CN113121360A (en) * | 2019-12-30 | 2021-07-16 | 青岛海湾精细化工有限公司 | Preparation method of scarlet base G |
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Application publication date: 20170104 |