CN104447411A - Refining method for normal-butyl isocyanate - Google Patents
Refining method for normal-butyl isocyanate Download PDFInfo
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- CN104447411A CN104447411A CN201410692026.7A CN201410692026A CN104447411A CN 104447411 A CN104447411 A CN 104447411A CN 201410692026 A CN201410692026 A CN 201410692026A CN 104447411 A CN104447411 A CN 104447411A
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- Prior art keywords
- butyl isocyanate
- butyl
- solution
- refined
- purification
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000007670 refining Methods 0.000 title abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 78
- 239000002253 acid Substances 0.000 claims abstract description 20
- 239000012044 organic layer Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- HNHVTXYLRVGMHD-UHFFFAOYSA-N n-butyl isocyanate Chemical compound CCCCN=C=O HNHVTXYLRVGMHD-UHFFFAOYSA-N 0.000 claims description 92
- 239000000243 solution Substances 0.000 claims description 61
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 36
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 20
- 238000000746 purification Methods 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- KLANNTYSNNUFQN-UHFFFAOYSA-N 1,2-xylene;hydrochloride Chemical compound Cl.CC1=CC=CC=C1C KLANNTYSNNUFQN-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 6
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 239000010410 layer Substances 0.000 abstract description 3
- 239000012074 organic phase Substances 0.000 abstract description 2
- 241000628997 Flos Species 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 229940100389 Sulfonylurea Drugs 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- YROXIXLRRCOBKF-UHFFFAOYSA-N sulfonylurea Chemical class OC(=N)N=S(=O)=O YROXIXLRRCOBKF-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a refining method of normal-butyl isocyanate. The method comprises the following steps: providing normal-butyl isocyanate solution to be refined, adding alchlor and dropwise adding a sodium hydroxide solution to the normal-butyl isocyanate solution to be refined at minus 10 to minus 5 DEG C while stirring, ensuring that reaction is performed for 0.5 to 1 hour, so as to obtain mixed liquor, ensuring that the mixed liquor is subjected to standing and layering, and separating and purifying an organic layer in the upper layer, so as to obtain the normal-butyl isocyanate. According to the refining method for normal-butyl isocyanate, impurity acid and a poly (normal-butyl isocyanate) floccule in the normal-butyl isocyanate to be refined are neutralized by using by the sodium hydroxide under the action of alchlor, then standing and layering are carried out, and the organic phase in the upper layer is separated and purified to obtain the normal-butyl isocyanate; according to the method, the product quality is improved.
Description
Technical field
The present invention relates to chemical field, particularly relate to a kind of process for purification of n-butyl isocyanate.
Background technology
N-butyl isocyanate is a kind of important pesticide intermediate.When phosgenation prepares sulfonylurea herbicide with n-butyl isocyanate as catalyzer, can reacting balance be made, improve yield; N-butyl isocyanate is also for the synthesis of agricultural bactericide F-1991.F-1991 is a kind of high-efficiency broad spectrum, systemic fungicide, has protection, roots out and therapeutic action, can prevent and treat various crop disease.But the n-butyl isocyanate produced of the synthetic method of traditional n-butyl isocyanate exist muddy, free acid is higher and be difficult to the problems such as removing, do not meet specification of quality, short term stored and auto-polymerization and form floss, subsequent reactions yield is reduced, affects quality product.
Summary of the invention
Based on this, be necessary the n-butyl isocyanate produced for the synthetic method of traditional n-butyl isocyanate exist muddy, free acid is higher and be difficult to the problem removed, provides a kind of process for purification of n-butyl isocyanate.
A process for purification for n-butyl isocyanate, comprises the following steps:
N-butyl isocyanate solution to be refined is provided;
At-10 DEG C ~-5 DEG C, add aluminum chloride in n-butyl isocyanate solution to be refined toward described in while stirring and drip sodium hydroxide solution, reacting 05 ~ 1 hour, obtain mixed solution; And
Described mixed solution is standing, layering, gets upper organic layer and carries out separating-purifying, obtain n-butyl isocyanate.
Wherein in an embodiment, the concentration of described sodium hydroxide solution is 0.2mol/L ~ 0.25mol/L.
Wherein in an embodiment, described in the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined be 1:0.05:5 ~ 6.
Wherein in an embodiment, described in the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined be 1:0.05:5.5.
Wherein in an embodiment, the time of described dropping sodium hydroxide solution is 0.5 ~ 1 hour.
Wherein in an embodiment, described mixed solution is left standstill, in the step of layering, the described standing time is 30 ~ 60 minutes.
Wherein in an embodiment, described in get upper organic layer and carry out separating-purifying, the step obtaining n-butyl isocyanate is specially: get upper organic layer and carry out underpressure distillation, collects cut, obtains n-butyl isocyanate.
Wherein in an embodiment, in the step of described underpressure distillation, the vacuum tightness≤-0.09MPa of underpressure distillation.
Wherein in an embodiment, described in n-butyl isocyanate solution to be refined provided by following steps:
By dimethylbenzene and n-Butyl Amine 99 mixing, drip hydrochloric acid, obtain the mixing solutions containing n-Butyl Amine 99 hydrochloride;
The described mixing solutions containing n-Butyl Amine 99 hydrochloride is heated, under reflux conditions azeotropic dehydration, until moisture is to the greatest extent de-, obtain n-Butyl Amine 99 hydrochloride dimethylbenzene material;
Described n-Butyl Amine 99 hydrochloride dimethylbenzene material is carried out logical phosgene reaction, obtains the mixture containing n-butyl isocyanate; And
The described mixture containing n-butyl isocyanate is carried out rectifying, n-butyl isocyanate solution to be refined described in obtaining.
Wherein in an embodiment, described in n-butyl isocyanate solution to be refined, mass content >=99.0% of n-butyl isocyanate, the mass content > 0.5% of impurity free acid.
The process for purification of above-mentioned n-butyl isocyanate, utilize sodium hydroxide under the effect of aluminum chloride, neutralize the impurity acid in n-butyl isocyanate to be refined and poly-n-butyl isocyanate floss, pass through stratification again, get upper organic phase and carry out separating-purifying, obtain n-butyl isocyanate, improve quality product.
Accompanying drawing explanation
Fig. 1 is the process for purification schematic flow sheet of the n-butyl isocyanate of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, be the process for purification of the n-butyl isocyanate of an embodiment, comprise the following steps:
S110, provide n-butyl isocyanate solution to be refined.
N-butyl isocyanate solution above-mentioned to be refined is provided by following steps: by dimethylbenzene and n-Butyl Amine 99 mixing, drip hydrochloric acid, obtain the mixing solutions containing n-Butyl Amine 99 hydrochloride; The above-mentioned mixed solution solution containing n-Butyl Amine 99 hydrochloride is heated, under reflux conditions azeotropic dehydration, until moisture is to the greatest extent de-, obtain n-Butyl Amine 99 hydrochloride dimethylbenzene material; Above-mentioned n-Butyl Amine 99 hydrochloride dimethylbenzene material is carried out logical phosgene reaction, obtains the mixture containing n-butyl isocyanate; Finally the above-mentioned mixture containing n-butyl isocyanate is carried out rectifying, obtain n-butyl isocyanate solution to be refined.
Concrete, by dimethylbenzene, n-Butyl Amine 99 by measuring header tank, quantitatively dropping into salt-forming reactor, drip hydrochloric acid in the cooling condition, produce the mixing solutions containing n-Butyl Amine 99 hydrochloride; Then by steam jacket heat temperature raising, azeotropic dehydration under reflux conditions, till taking off to the greatest extent by moisture, obtains n-Butyl Amine 99 hydrochloride dimethylbenzene material; By n-Butyl Amine 99 hydrochloride dimethylbenzene material press-in photochmeical reaction pot, under reflux conditions, carry out logical phosgene reaction, until n-Butyl Amine 99 hydrochloride is all converted into n-butyl isocyanate, then catch up with light, the mixture obtained containing n-butyl isocyanate supplies rectifying separation; Finally the above-mentioned mixture containing n-butyl isocyanate is added rectifying tower, carry out total reflux to tower top with high temperature heat conductive oil heating, obtain n-butyl isocyanate solution to be refined.
In isocyanate solution above-mentioned to be refined, mass content >=99.0% of n-butyl isocyanate, the mass content > 0.5% of impurity free acid.
Be appreciated that, n-butyl isocyanate solution above-mentioned to be refined is not limited to above step to be provided, as long as mass content >=99.0% of the n-butyl isocyanate produced, the mass content > 0.5% of impurity free acid can adopt process for purification herein to refine.
S120, at-10 DEG C ~-5 DEG C, add in n-butyl isocyanate solution above-mentioned to be refined while stirring aluminum chloride and drip sodium hydroxide solution, react 0.5 ~ 1 hour, obtain mixed solution.
Wherein, the concentration of sodium hydroxide solution is 0.2mol/L ~ 0.25mol/L.
The time dripping sodium hydroxide solution is 0.5 ~ 1 hour.
In the step s 120, the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined is 1:0.05:5 ~ 6.
Preferably, the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined is 1:0.05:5.5.
Due to the katalysis of aluminum chloride, impurity free acid and cotton-shaped muddy thing and sodium hydroxide thoroughly react, and improve quality product.
S130, above-mentioned mixed solution is standing, layering, get upper organic layer and carry out separating-purifying, obtain n-butyl isocyanate.
Wherein, the time left standstill is 30 ~ 60 minutes.
Get upper organic layer and carry out separating-purifying, the step obtaining n-butyl isocyanate is specially: get upper organic layer and carry out underpressure distillation, collects cut, obtains n-butyl isocyanate.
Wherein, the vacuum tightness≤-0.09MPa of underpressure distillation.
It should be noted that, above-mentioned mixed solution leave standstill, layering, the lower floor's inorganic layer obtained by sewage plant harmless treatment, without waste water and gas produce, pollute lack, safety and environmental protection.
The process for purification of above-mentioned n-butyl isocyanate, under the effect of catalyzer aluminum chloride, impurity free acid contained in n-butyl isocyanate solution to be refined and poly-n-butyl isocyanate floss is neutralized with sodium hydroxide, can by impurity free acid and floss separating-purifying, and the normal-butyl cyanate steady quality after purifying, can standing storage never degenerate.
It is below specific embodiment.
Embodiment 1
There is provided n-butyl isocyanate solution 500L to be refined, by analysis, the mass content of n-butyl isocyanate is 99.1%, and the mass content of free acid is 0.69%, and there is a large amount of White Flocculus the inside.
At-8 DEG C, add aluminum chloride toward n-butyl isocyanate solution above-mentioned to be refined while stirring and drip the sodium hydroxide solution of 0.2mol/L, react 1 hour, obtain mixed solution, the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution wherein to be refined is 1:0.05:5.5.
Above-mentioned mixed solution is left standstill 60 minutes, gets upper organic layer and carry out underpressure distillation, collect cut, obtain 480L sample.By analysis, in sample, the mass content of n-butyl isocyanate is 99.63%, and the mass content of free acid is 0.09%, and clear appearance is transparent; The mass content that n-butyl isocyanate after 7 days placed by sample is 99.61%, and the mass content of free acid is 0.09%, and clear appearance is transparent, without flocculent substance.
Embodiment 2
There is provided n-butyl isocyanate solution 1000L to be refined, by analysis, the mass content of n-butyl isocyanate is 99.21%, and the mass content of free acid is 0.75%, and there is a large amount of White Flocculus the inside.
At-10 DEG C, add aluminum chloride toward n-butyl isocyanate solution above-mentioned to be refined while stirring and drip the sodium hydroxide solution of 0.23mol/L, react 1 hour, obtain mixed solution, the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution wherein to be refined is 1:0.05:5.
Above-mentioned mixed solution is left standstill 30 minutes, gets upper organic layer and carry out underpressure distillation, collect cut, obtain 985L sample.By analysis, in sample, the mass content of n-butyl isocyanate is 99.7%, and the mass content of free acid is 0.06%, and clear appearance is transparent; The mass content that n-butyl isocyanate after 14 days placed by sample is 99.69%, and the mass content of free acid is 0.06%, and clear appearance is transparent, without flocculent substance.
Embodiment 3
There is provided n-butyl isocyanate solution 1500L to be refined, by analysis, the mass content of n-butyl isocyanate is 99.23%, and the mass content of free acid is 0.72%, and there is a large amount of White Flocculus the inside.
At-7 DEG C, add aluminum chloride toward n-butyl isocyanate solution above-mentioned to be refined while stirring and drip the sodium hydroxide solution of 0.25mol/L, react 1 hour, obtain mixed solution, the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution wherein to be refined is 1:0.05:5.5.
Above-mentioned mixed solution is left standstill 45 minutes, gets upper organic layer and carry out underpressure distillation, collect cut, obtain 1480L sample.By analysis, in sample, the mass content of n-butyl isocyanate is 99.78%, and the mass content of free acid is 0.04%, and clear appearance is transparent; Placing the mass content of n-butyl isocyanate after 28 days is 99.75%, and the mass content of free acid is 0.05%, and clear appearance is transparent, without flocculent substance.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a process for purification for n-butyl isocyanate, is characterized in that, comprises the following steps:
N-butyl isocyanate solution to be refined is provided;
At-10 DEG C ~-5 DEG C, add aluminum chloride in n-butyl isocyanate solution to be refined toward described in while stirring and drip sodium hydroxide solution, reacting 0.5 ~ 1 hour, obtain mixed solution; And
Described mixed solution is standing, layering, gets upper organic layer and carries out separating-purifying, obtain n-butyl isocyanate.
2. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, the concentration of described sodium hydroxide solution is 0.2mol/L ~ 0.25mol/L.
3. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, described in the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined be 1:0.05:5 ~ 6.
4. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, described in the mass ratio of n-butyl isocyanate solution, aluminum chloride and sodium hydroxide solution to be refined be 1:0.05:5.5.
5. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, the time of described dropping sodium hydroxide solution is 0.5 ~ 1 hour.
6. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, is left standstill by described mixed solution, in the step of layering, the described standing time is 30 ~ 60 minutes.
7. the process for purification of n-butyl isocyanate according to claim 1, it is characterized in that, described in get upper organic layer and carry out separating-purifying, the step obtaining n-butyl isocyanate is specially: get upper organic layer and carry out underpressure distillation, collect cut, obtain n-butyl isocyanate.
8. the process for purification of n-butyl isocyanate according to claim 7, is characterized in that, in the step of described underpressure distillation, and the vacuum tightness≤-0.09MPa of underpressure distillation.
9. the process for purification of n-butyl isocyanate according to claim 1, is characterized in that, described in n-butyl isocyanate solution to be refined provided by following steps:
By dimethylbenzene and n-Butyl Amine 99 mixing, drip hydrochloric acid, obtain the mixing solutions containing n-Butyl Amine 99 hydrochloride;
The described mixing solutions containing n-Butyl Amine 99 hydrochloride is heated, under reflux conditions azeotropic dehydration, until moisture is to the greatest extent de-, obtain n-Butyl Amine 99 hydrochloride dimethylbenzene material;
Described n-Butyl Amine 99 hydrochloride dimethylbenzene material is carried out logical phosgene reaction, obtains the mixture containing n-butyl isocyanate; And
The described mixture containing n-butyl isocyanate is carried out rectifying, n-butyl isocyanate solution to be refined described in obtaining.
10. the process for purification of n-butyl isocyanate according to claim 1, it is characterized in that, in n-butyl isocyanate solution described to be refined, mass content >=99.0% of n-butyl isocyanate, the mass content > 0.5% of impurity free acid.
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| CN201410692026.7A CN104447411B (en) | 2014-11-27 | 2014-11-27 | The process for purification of n-butyl isocyanate |
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| CN201410692026.7A CN104447411B (en) | 2014-11-27 | 2014-11-27 | The process for purification of n-butyl isocyanate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384659A (en) * | 2015-10-26 | 2016-03-09 | 安徽广信农化股份有限公司 | Method for synthesizing n-butyl isocyanate |
| CN110218163A (en) * | 2019-05-20 | 2019-09-10 | 江苏蓝丰生物化工股份有限公司 | The synthetic method of n-butyl isocyanate |
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| US4094894A (en) * | 1977-03-23 | 1978-06-13 | E. I. Du Pont De Nemours And Company | Process of purifying aliphatic isocyanates |
| EP1046636A2 (en) * | 1999-03-30 | 2000-10-25 | Bayer Ag | Process for the reduction of chlorine content of organic isocyanates |
| CN1844091A (en) * | 2006-05-08 | 2006-10-11 | 江苏安邦电化有限公司 | Process for preparing butyl isocyanate |
| CN101084187A (en) * | 2004-12-22 | 2007-12-05 | 朗盛德国有限责任公司 | Method for the reduction of chlorine-containing components in organic isocyanates |
| CN103638688A (en) * | 2013-12-24 | 2014-03-19 | 湖南国发精细化工科技有限公司 | Recycling method for phosgene in tail gas generated in calorescence reaction for synthesizing normal-butyl isocyanate |
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2014
- 2014-11-27 CN CN201410692026.7A patent/CN104447411B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4094894A (en) * | 1977-03-23 | 1978-06-13 | E. I. Du Pont De Nemours And Company | Process of purifying aliphatic isocyanates |
| EP1046636A2 (en) * | 1999-03-30 | 2000-10-25 | Bayer Ag | Process for the reduction of chlorine content of organic isocyanates |
| EP1046636A3 (en) * | 1999-03-30 | 2002-06-19 | Bayer Ag | Process for the reduction of chlorine content of organic isocyanates |
| CN101084187A (en) * | 2004-12-22 | 2007-12-05 | 朗盛德国有限责任公司 | Method for the reduction of chlorine-containing components in organic isocyanates |
| CN1844091A (en) * | 2006-05-08 | 2006-10-11 | 江苏安邦电化有限公司 | Process for preparing butyl isocyanate |
| CN103638688A (en) * | 2013-12-24 | 2014-03-19 | 湖南国发精细化工科技有限公司 | Recycling method for phosgene in tail gas generated in calorescence reaction for synthesizing normal-butyl isocyanate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105384659A (en) * | 2015-10-26 | 2016-03-09 | 安徽广信农化股份有限公司 | Method for synthesizing n-butyl isocyanate |
| CN110218163A (en) * | 2019-05-20 | 2019-09-10 | 江苏蓝丰生物化工股份有限公司 | The synthetic method of n-butyl isocyanate |
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| CN104447411B (en) | 2016-10-05 |
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Application publication date: 20150325 Assignee: Hunan Weimo New Material Co.,Ltd. Assignor: HUNAN GOFAR FINE CHEMICAL TECH. CO.,LTD. Contract record no.: X2023980047358 Denomination of invention: Refining method of n-butyl isocyanate Granted publication date: 20161005 License type: Common License Record date: 20231120 |
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