CN109851472A - A kind of production technology of high-purity 2,4-DCT - Google Patents
A kind of production technology of high-purity 2,4-DCT Download PDFInfo
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- CN109851472A CN109851472A CN201811577759.0A CN201811577759A CN109851472A CN 109851472 A CN109851472 A CN 109851472A CN 201811577759 A CN201811577759 A CN 201811577759A CN 109851472 A CN109851472 A CN 109851472A
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Abstract
The present invention relates to compound synthesis technical field of purification, and in particular to a kind of production technology of high-purity 2,4-DCT.Include the following steps: to catalyze and synthesize 2,4-DCT using p-chlorotoluene and chlorine, is obtaining the 2,4-DCT of high-purity by alkali cleaning, rectifying recycling fraction, purified crystals.The present invention solves the problems, such as that 2,4-DCT low yield, purity are low in the prior art and are not easily purified, and the 2,4-DCT being prepared has the advantages that high yield, purity is high and material recoverable.
Description
Technical field
The present invention relates to compound synthesis technical field of purification, and in particular to a kind of production of high-purity 2,4-DCT
Technique.
Background technique
2,4-DCT is medicine or dyestuff intermediate CAS 95-73-8, and 2,4-DCT is colorless and transparent
Liquid；2,4-DCT is toxic, and rat oral LD50 is 4640mg/kg.Operationlocation pays attention to well-ventilated, and equipment is closed,
Operator dresses safety device.2,4-DCT meets open fire burning, should store at shady and cool ventilation, keep fire away, heat source, with
Oxidant is separately stored, and with food, feed, seed is separately stored, and pays attention to keeping Packing Intact.
2,4-dichlorotoleune are highly important organic synthesis fine-chemical intermediates, can be used for synthesizing 2,4-dichloros
Benzoic acid, 2,4-benzyl dichlorides, 2,4-dichloro acyl chlorides and 2, a variety of Organic chemical products such as 4-dichlorobenzaldehydes, are pesticides
The primary raw material of pyrazolate (herbicide), olefin conversion (fungicide), medical Ciprofloxacin etc..
In the prior art, impurity is more in the chloride for using p-chlorotoluene and ortho-chlorotolu'ene to generate for raw material, and boiling point
Close, the fractionation of Yao Caiyong high-efficient spiral-screen column can just obtain 98% or more 2,4-DCT.It is original with p-chlorotoluene, chlorine
Material synthesizes in batch still in the presence of Lewis acid.The selectivity of this method 2,4-dichlorotoleune in the industrial production
Lower, by-product is more, acid waste water is more, catalyst consumption is big.It is made by the isomerization of dichlorotoleune, in isomerized products utilization
Porous molecular sieve separation.The production cost of this method is higher, and industrial production is difficult.Using 3- chlorine para-totuidine as raw material, with nitrous acid
Sodium carries out diazo-reaction, has obtained the salt of the chloro- 4- diazonium ylmethyl of 2-, by diazo-group convertion is chlorine with stannous chloride, through point
From purification, 2,4-dichlorotoleune are obtained.This method complex process, product yield are low.Using p-chlorotoluene, chlorine as raw material, with
NaKL zeolite catalyst, a step direct chlorination synthesizes 2,4-dichlorotoleune in fixed bed continuous reactor.Though this method technique
Simply, the three wastes are few, but the conversion ratio of p-chlorotoluene and 2, and the rate of 4-dichlorotoleune is lower, and only 55% or so.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of production works of high-purity 2,4-DCT
Skill solves the problems, such as 2, the 4- bis- that 2,4-DCT low yield, purity are low in the prior art and are not easily purified, and are prepared
Chlorotoluene has the advantages that high yield, purity is high and material recoverable.
The purpose of the present invention is achieved through the following technical solutions:
A kind of production technology of high-purity 2,4-DCT, includes the following steps:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and catalyst are added in reaction vessel, temperature be 40 ~
Chlorine is passed through at 41 DEG C again, stopping at least being reacted 30min after being passed through chlorine, stood at least after adding purified water absorbing hydrogen chloride
30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and organic solvent, stands at least 15min, isolated organic layer, vacuum distillation recycling
It is stand-by to obtain residue for organic solvent；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune.
React at least 30min after the completion of being passed through chlorine, improve the conversion ratio of chlorine, chlorine to be passed through speed smaller,
Reaction speed is reduced, avoids producing excessive polychloride, avoids the generation of side reaction, avoid the reduction of reaction yield；Reaction
The hydrogen chloride of generation is absorbed using water generates hydrochloric acid solution, and recoverable increases the utilization rate of material.
It is layered after alkali cleaning using water phase and organic phase, isolated organic phase carries out rectifying, in distillation process
It is middle first by the fraction collection recycling and reusing of p-chlorotoluene, the boiling point of p-chlorotoluene differs larger with 2,4-DCT, can obtain
It is used as the raw material of chlorination reaction to use again to the higher p-chlorotoluene of purity, improves conversion ratio and the utilization of p-chlorotoluene
Rate；During 2,4-DCT fraction collection, selects shorter boiling range to be collected, obtain higher 2, the 4- bis- of purity
Chlorotoluene；Again by 2,4-DCT crystallization purifying again, obtained 2,4-DCT purity >=99.9%.
Further, the molar ratio of p-chlorotoluene and chlorine is 1:(1.3 ~ 1.5 in the step 1)；In the step 1
Purified water and the molar ratio of p-chlorotoluene are 1:(3.0 ~ 4.0).
It is further preferred that the molar ratio of p-chlorotoluene and chlorine is 1:1.4 in the step 1；It is pure in the step 1
The molar ratio for changing water and p-chlorotoluene is 1:4.0.
Further, the step 1 catalyst is NaKL zeolite；In the step 1 chlorine be passed through speed be 0.6 ~
0.8L/min。
2,4-DCT in above-mentioned technique have=simple process, raw material are easy to get, side reaction is few, product quality is high,
The advantage that product yield is high, alkali cleaning effect is good, environmental pollution is small, rectification yield is high and product purity is high；By chlorination reaction
Temperature is controlled at 40 ~ 41 DEG C, is improved the yield that p-chlorotoluene is changed into 2,4-DCT, is reduced the generation of side reaction.
Further, in the step 2 alkaline residue be calcium carbonate, magnesium carbonate, magnesium hydroxide and/or calcium hydroxide in extremely
Few one kind.
Further, the volume ratio of purified water in the step 2, organic solvent and the organic liquid mixture be 1:(0.9 ~
1.1): (0.3 ~ 0.5).
It is further preferred that the volume ratio of purified water, organic solvent and the organic liquid mixture is 1 in the step 2:
1.0:0.4.
Further, the organic solvent is ether or methylene chloride.
Further, in the step 4 2,4-DCT decrease temperature crystalline pressure be 0.30 ~ 0.32MPz, temperature be-
5~ 5℃。
Further, the pressure of steam insulation is 0.30 ~ 0.35MPa in the step 4, and temperature is 80 ~ 100 DEG C.
The beneficial effects of the present invention are:
1.2,4- dichlorotoleune in above-mentioned technique have=simple process, raw material are easy to get, side reaction is few, product quality is high, produce
The advantage that product high income, alkali cleaning effect are good, environmental pollution is small, rectification yield is high and product purity is high；By the temperature of chlorination reaction
Degree control improves the yield that p-chlorotoluene is changed into 2,4-DCT, reduces the generation of side reaction at 40 ~ 41 DEG C；
2. react at least 30min after the completion of being passed through chlorine, the conversion ratio of chlorine is improved, smaller, the drop that is passed through speed of chlorine
Low reaction speed avoids producing excessive polychloride, avoids the generation of side reaction, avoids the reduction of reaction yield；Reaction life
At hydrogen chloride absorbed using water and generate hydrochloric acid solution, recoverable increases the utilization rate of material；
3. being layered after alkali cleaning using water phase and organic phase, isolated organic phase carries out rectifying, in distillation process
First by the fraction collection recycling and reusing of p-chlorotoluene, the boiling point of p-chlorotoluene differs larger with 2,4-DCT, can be obtained
The higher p-chlorotoluene of purity is used as the raw material of chlorination reaction to use again, improves the conversion ratio and utilization rate of p-chlorotoluene；
During 2,4-DCT fraction collection, selects shorter boiling range to be collected, obtain higher 2, the 4- dichloro of purity
Toluene；Again by 2,4-DCT crystallization purifying again, obtained 2,4-DCT purity >=99.9%.
Specific embodiment
Technical solution of the present invention is described in further detail combined with specific embodiments below, but protection scope of the present invention is not
It is confined to as described below.
Embodiment 1
A kind of production technology of high-purity 2,4-DCT, includes the following steps:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and NaKL zeolite being added in reaction vessel, are 40 in temperature
Chlorine is passed through at DEG C again, stopping at least being reacted 30min after being passed through chlorine, stood at least after adding purified water absorbing hydrogen chloride
30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture, wherein to chloromethane
The molar ratio of benzene and chlorine is 1:1.3, and the molar ratio of purified water and p-chlorotoluene is 1:3.0, and the speed that is passed through of chlorine is 0.6L/
min；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and ether or methylene chloride, stands at least 15min, isolated organic layer, and decompression is steamed
Recycling organic solvent is evaporated, obtains that residue is stand-by, wherein the volume ratio of purified water, organic solvent and the organic liquid mixture is 1:
0.9:0.3；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune, wherein the pressure of 2,4-DCT decrease temperature crystalline is 0.30MPz, and temperature is -5 ~ 5 DEG C；The pressure of steam insulation
For 0.30MPa, temperature is 80 ~ 100 DEG C.
Specifically, alkaline residue is calcium carbonate in the step 2；The organic solvent is ether.
After the 2,4-DCT rectifying that above-described embodiment is prepared with p-chlorotoluene note yield be 68%, after purification with
P-chlorotoluene remembers that yield is 67%, and purity is 99.9% after purification.
Embodiment 2
A kind of production technology of high-purity 2,4-DCT, includes the following steps:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and NaKL zeolite being added in reaction vessel, are 41 in temperature
Chlorine is passed through at DEG C again, stopping at least being reacted 30min after being passed through chlorine, stood at least after adding purified water absorbing hydrogen chloride
30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture, wherein to chloromethane
The molar ratio of benzene and chlorine is 1:1.5, and the molar ratio of purified water and p-chlorotoluene is 1:4.0, and the speed that is passed through of chlorine is 0.8L/
min；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and ether or methylene chloride, stands at least 15min, isolated organic layer, and decompression is steamed
Recycling organic solvent is evaporated, obtains that residue is stand-by, wherein the volume ratio of purified water, organic solvent and the organic liquid mixture is 1:
1.1:0.5；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune, wherein the pressure of 2,4-DCT decrease temperature crystalline is 0.32MPz, and temperature is -5 ~ 5 DEG C；The pressure of steam insulation
For 0.35MPa, temperature is 80 ~ 100 DEG C.
Specifically, alkaline residue is calcium hydroxide in the step 2；The organic solvent is methylene chloride.
After the 2,4-DCT rectifying that above-described embodiment is prepared with p-chlorotoluene note yield be 67%, after purification with
P-chlorotoluene remembers that yield is 66%, and purity is 99.9% after purification.
Embodiment 3
A kind of production technology of high-purity 2,4-DCT, includes the following steps:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and NaKL zeolite being added in reaction vessel, are 40 in temperature
Chlorine is passed through at DEG C again, stopping at least being reacted 30min after being passed through chlorine, stood at least after adding purified water absorbing hydrogen chloride
30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture, wherein to chloromethane
The molar ratio of benzene and chlorine is 1:1.4, and the molar ratio of purified water and p-chlorotoluene is 1:3.5, and the speed that is passed through of chlorine is 0.7L/
min；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and ether or methylene chloride, stands at least 15min, isolated organic layer, and decompression is steamed
Recycling organic solvent is evaporated, obtains that residue is stand-by, wherein the volume ratio of purified water, organic solvent and the organic liquid mixture is 1:
1.0:0.4；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune, wherein the pressure of 2,4-DCT decrease temperature crystalline is 0.31MPz, and temperature is -5 ~ 5 DEG C；The pressure of steam insulation
For 0.32MPa, temperature is 80 ~ 100 DEG C.
Specifically, alkaline residue is magnesium hydroxide in the step 2；The organic solvent is ether.
After the 2,4-DCT rectifying that above-described embodiment is prepared with p-chlorotoluene note yield be 68%, after purification with
P-chlorotoluene remembers that yield is 67%, and purity is 99.9% after purification.
Embodiment 4
A kind of production technology of high-purity 2,4-DCT, includes the following steps:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and NaKL zeolite being added in reaction vessel, are 40 in temperature
Be passed through chlorine at ~ 41 DEG C again, stopping at least reacting 30min after being passed through chlorine, add after purified water absorbing hydrogen chloride stand to
Few 30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture, wherein to chlorine
The molar ratio of toluene and chlorine is 1:1.4, and the molar ratio of purified water and p-chlorotoluene is 1:4.0, and the speed that is passed through of chlorine is
0.6L/min；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and ether or methylene chloride, stands at least 15min, isolated organic layer, and decompression is steamed
Recycling organic solvent is evaporated, obtains that residue is stand-by, wherein the volume ratio of purified water, organic solvent and the organic liquid mixture is 1:
1.0:0.4；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune, wherein the pressure of 2,4-DCT decrease temperature crystalline is 0.31MPz, and temperature is -5 ~ 5 DEG C；The pressure of steam insulation
For 0.33MPa, temperature is 80 ~ 100 DEG C.
Specifically, in the step 2 alkaline residue be calcium carbonate, magnesium carbonate, magnesium hydroxide and/or calcium hydroxide at least
It is a kind of；The organic solvent is ether or methylene chloride.
After the 2,4-DCT rectifying that above-described embodiment is prepared with p-chlorotoluene note yield be 69%, after purification with
P-chlorotoluene remembers that yield is 68%, and purity is 99.9% after purification.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection scope of appended claims of the present invention
It is interior.
Claims (10)
1. a kind of production technology of high-purity 2,4-DCT, which comprises the steps of:
Step 1: catalyzing and synthesizing 2,4-DCT: p-chlorotoluene and catalyst are added in reaction vessel, temperature be 40 ~
Chlorine is passed through at 41 DEG C again, stopping at least being reacted 30min after being passed through chlorine, stood at least after adding purified water absorbing hydrogen chloride
30min obtains hydrochloric acid solution, recycles hydrochloric acid solution by HCl recovery device, it is stand-by to obtain organic liquid mixture；
Step 2: alkali cleaning: alkaline residue being added in the organic liquid mixture into step 1 and carries out alkali cleaning, is filtered to remove alkaline residue, adds
Concussion at least 5min is rocked after purified water and organic solvent, stands at least 15min, isolated organic layer, vacuum distillation recycling
It is stand-by to obtain residue for organic solvent；
Step 3: rectifying: residue is added in rectifying column and carry out rectifying, 162 ~ 165 DEG C of fraction is recycled, regather 200 ~
It is stand-by to obtain crude 2,4-DCT for 202 DEG C of fraction；
Step 4: purifying: 2,4-DCT crude in step 3 being added in the jacket reactor equipped with refrigerating coil, is opened
The chilled brine valve for opening collet and refrigerating coil is passed through chilled brine and makes in reaction kettle 2,4-DCT decrease temperature crystalline extremely
Few 2h, closes the chilled brine valve of collet and refrigerating coil, then by negative pressure from the bottom valve of reaction kettle by liquid in reaction kettle
Extraction, closes the bottom valve of reaction kettle, rethinks and be passed through steam insulation at least 15min in the collet of reaction kettle to get high-purity 2,4-
Dichlorotoleune.
2. a kind of production technology of high-purity 2,4-DCT according to claim 1, which is characterized in that the step
The molar ratio of p-chlorotoluene and chlorine is 1:(1.3 ~ 1.5 in one)；The molar ratio of purified water and p-chlorotoluene in the step 1
For 1:(3.0 ~ 4.0).
3. a kind of production technology of high-purity 2,4-DCT according to claim 1, which is characterized in that the step
The molar ratio of p-chlorotoluene and chlorine is 1:1.4 in one；Purified water and the molar ratio of p-chlorotoluene are 1 in the step 1:
4.0。
4. the production technology of described in any item a kind of high-purity 2,4-DCTs according to claim 1 ~ 3, which is characterized in that
The step 1 catalyst is NaKL zeolite；The speed that is passed through of chlorine is 0.6 ~ 0.8L/min in the step 1.
5. a kind of production technology of high-purity 2,4-DCT according to claim 1, which is characterized in that the step
Alkaline residue is at least one of calcium carbonate, magnesium carbonate, magnesium hydroxide and/or calcium hydroxide in two.
6. a kind of production technology of high-purity 2,4-DCT according to claim 1 or 5, which is characterized in that described
The volume ratio of purified water, organic solvent and the organic liquid mixture is 1:(0.9 ~ 1.1 in step 2): (0.3 ~ 0.5).
7. a kind of production technology of high-purity 2,4-DCT according to claim 6, which is characterized in that the step
The volume ratio of purified water, organic solvent and the organic liquid mixture is 1:1.0:0.4 in two.
8. a kind of production technology of high-purity 2,4-DCT according to claim 6, which is characterized in that described organic
Solvent is ether or methylene chloride.
9. a kind of production technology of high-purity 2,4-DCT according to claim 1, which is characterized in that the step
The pressure of 2,4-DCT decrease temperature crystalline is 0.30 ~ 0.32MPz in four, and temperature is -5 ~ 5 DEG C.
10. according to claim 1 or a kind of production technology of high-purity 2,4-DCT described in 9, which is characterized in that described
The pressure of steam insulation is 0.30 ~ 0.35MPa in step 4, and temperature is 80 ~ 100 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546443A (en) * | 2003-12-11 | 2004-11-17 | 株洲化工集团诚信有限公司 | Method for preparing 2,4-toluene dichloride |
| CN105367381A (en) * | 2015-12-01 | 2016-03-02 | 南京钟腾化工有限公司 | Method for producing 2,4-dichlorotoluene by using parachlorotoluene |
| CN106242940A (en) * | 2016-08-01 | 2016-12-21 | 南京钟腾化工有限公司 | A kind of synthesis technique of 2,4 dichlorotoleune |
-
2018
- 2018-12-24 CN CN201811577759.0A patent/CN109851472A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546443A (en) * | 2003-12-11 | 2004-11-17 | 株洲化工集团诚信有限公司 | Method for preparing 2,4-toluene dichloride |
| CN105367381A (en) * | 2015-12-01 | 2016-03-02 | 南京钟腾化工有限公司 | Method for producing 2,4-dichlorotoluene by using parachlorotoluene |
| CN106242940A (en) * | 2016-08-01 | 2016-12-21 | 南京钟腾化工有限公司 | A kind of synthesis technique of 2,4 dichlorotoleune |
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Application publication date: 20190607 |