CN106395861A - Method for producing cyanogen chloride by using tubular reactor - Google Patents
Method for producing cyanogen chloride by using tubular reactor Download PDFInfo
- Publication number
- CN106395861A CN106395861A CN201610780155.0A CN201610780155A CN106395861A CN 106395861 A CN106395861 A CN 106395861A CN 201610780155 A CN201610780155 A CN 201610780155A CN 106395861 A CN106395861 A CN 106395861A
- Authority
- CN
- China
- Prior art keywords
- tubular reactor
- temperature
- reaction
- cyanogen chloride
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- QPJDMGCKMHUXFD-UHFFFAOYSA-N cyanogen chloride Chemical compound ClC#N QPJDMGCKMHUXFD-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 14
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- MNWBNISUBARLIT-UHFFFAOYSA-N sodium cyanide Chemical compound [Na+].N#[C-] MNWBNISUBARLIT-UHFFFAOYSA-N 0.000 claims description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000003795 desorption Methods 0.000 abstract 3
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000543 intermediate Substances 0.000 abstract 1
- 238000005660 chlorination reaction Methods 0.000 description 7
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- BECUGVVIKYMAHP-UHFFFAOYSA-N N#CC#N.N#CC#N.[Cl] Chemical compound N#CC#N.N#CC#N.[Cl] BECUGVVIKYMAHP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NCSHGROOCJHAFK-UHFFFAOYSA-N [Cl].N#CC#N Chemical compound [Cl].N#CC#N NCSHGROOCJHAFK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000834 fixative Substances 0.000 description 1
- 239000006081 fluorescent whitening agent Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/004—Halogenides of cyanogen
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of the synthesis of fine chemical intermediates, particularly relates to the technical field of the production of cyanogen chloride, and discloses a method for producing the cyanogen chloride by using a tubular reactor. The method comprises the following steps of mixing liquid chlorine with a sodium cyanide aqueous solution according to the mole ratio of sodium cyanide to the liquid chlorine, which is 1 to (0.9 to 1.2), controlling the temperature of obtained mixed liquor to be 20 to 50 DEG C, afterwards, introducing the mixed liquor into the tubular reactor to react, controlling the pressure of the tubular reactor to be 0.1MPa to 2.0MPa, and controlling reaction temperature to be 20 to 60 DEG C, wherein the residence time of the reaction is 10s to 600s; discharging material liquid after the completion of the reaction into a desorption tower from the tail end of the tubular reactor, and controlling the temperature of the desorption tower to be 20 to 60 DEG C, so as to obtain a pure cyanogen chloride gas through desorption and drying. By using the method provided by the invention, the production efficiency can be improved; the method has the advantages that the production yield is high and further the reactor is simple.
Description
Technical field
The present invention relates to fine-chemical intermediate synthesis technical field, especially relate to the production technical field of cyanogen chloride.
Background technology
Cyanogen chloride is the intermediate producing Cyanuric Chloride, mainly for the production of Cyanuric Chloride, diphenylguanidine, dicyandiamide sodium, washes
Must the fine-chemical intermediate such as Thailand, wherein Cyanuric Chloride is widely used in chemical field, is many pesticide, herbicide, work
Property dyestuff and the important source material of fluorescent whitening agent.Meanwhile, cyanogen chloride can also be used for producing nitrogen fertilizer potentiating agent, surfactant, increasing
Fast agent, stabilizer, thiofide, polymer foaming agent, resin fixative, polymerization catalyst, fireproof agent, photosensitive
Agent, binding agent, cyanaldehyde resin, reverse osmotic membrane, stability gunpowder and multi-medicament.
At present, countries in the world mainly adopt wet chlorination two-step method to produce Cyanuric Chloride, about patent description in this respect
More, such as USP3499737, USP3535091, USP35674056, USp3755542, USP3535090, USP4100263,
USP39474199, USP3825658 etc..After the method is carried out wet chlorination, is separated, is dehydrated, being polymerized, sublimate by HCN and Cl2
The processes such as reason composition.
Cyanogran. chlorination reaction is using special gaseous mixture stream nozzle, makes sodium cyanide solution and chlorine in spray form
Under state, direct reaction generates chlorine cyanogen.At present, domestic common using this method.Its advantage is that available commercial sodium cyanide is configured to water
Solution, need not adjust pH value and go deimpurity operation sequence process route short, the simple final product of operating procedure can be immediately
Separated by reactant mixture, purity is preferable, but shortcoming is that spraying control requirement is strict, gas-liquid mixed effect hardly possible controls.
《Liaoning chemical industry》In in November, 2015 volume 44 o. 11th, " Cyanuric Chloride produces the research and development of chlorination reaction new technology " describes
Reacted using thtee-stage shiplock and ensure that raw material reaction is thorough, it is to avoid the defect of high-temperature chlorization craft and low temperature chlorination technique, but
Equipment is complicated, operating difficultiess.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of method of use tubular reactor produced cyanogen chloride, tool
There are production high income and the simple advantage of reactor.
For solving above-mentioned technical problem, the technical solution used in the present invention is：One kind uses tubular reactor produced chlorine
The method changing cyanogen, including：It is 1 that liquid chlorine and sodium cyanide solution are pressed Cyanogran. and liquid chlorine mol ratio：0.9～1.2 ratio is mixed
Close, and control its temperature at 20～50 DEG C, then mixed liquor is passed through reaction in tubular reactor, controls tubular type reactor pressure
0.1～2.0MPa, reaction temperature controls at 20～60 DEG C, and reaction time is 10～600s；
Feed liquid after the completion of reaction is entered Analytic Tower from the tail end of tubular reactor, the temperature control of Analytic Tower is 20～60
DEG C, through parsing, it is dried to obtain pure cyanogen chloride gas.
Analytic Tower of the present invention is knockout tower, for gas-liquid separation.Preferably, in knockout tower along tower body from top to bottom
Temperature is gradually lowered, and cyanogen chloride gas can be enriched in tower top and produce, chlorination saline converges at tower reactor and produces.
Further, described sodium cyanide solution is 30% sodium cyanide solution, and it is with liquid chlorine respectively through liquid feedstock
Pumping material, and after respective effusion meter accurate flow adjustment, enter blender mixing, control feed liquid temperature at mixer outlet
Degree is at 20～50 DEG C.
Preferably, controlling tubular type reactor pressure 0.4～1.5MPa.
As it is further preferred that controlling tubular type reactor pressure 0.6～1.0MPa.
Preferably, reaction time is 20～300s.
Have the beneficial effects that using produced by technique scheme：The present invention is using liquid chlorine, sodium cyanide solution as former
Material, prepares cyanogen chloride by tubular reactor, reactant liquor enters directly into Analytic Tower from the tail end of tubular reactor and parsed,
Improve production efficiency, simplify consersion unit, reduce fixed assets investment, simple to operate, and high conversion rate reach 99% with
On, there is certain economic and social benefit.
Brief description
Fig. 1 is a kind of process chart of the inventive method.
Wherein, 1, effusion meter；2nd, blender；3rd, tubular reactor；4th, Analytic Tower；5th, extraction-container.
Described blender and tubular reactor all control the temperature of feed liquid by recirculated water；The end of tubular reactor with
The charging aperture on Analytic Tower top connects, and the saline extraction of the chloride containing cyanogen of Analytic Tower bottom is sent in extraction-container, controls extraction-container
Temperature be 90～100 DEG C, Isolating chlorinated cyanogen again, remaining chlorination saline go wastewater treatment working section process.Analytic Tower is sky
Tower is simultaneously provided with temperature-reducing coil, as the space of gas-liquid separation.
Specific embodiment
Following instance is used for further describing a kind of method of use tubular reactor produced cyanogen chloride.But the present invention
It is only limitted to absolutely not following instance.The side that tubular reactor in claim limited range all can provide according to the present invention
Method is used for preparing cyanogen chloride.
Following examples are all using technological process shown in Fig. 1.
Embodiment 1
（1）After intelligent flow meter accurate flow adjustment, liquid chlorine flow-control in 0.25t/h, 30% sodium cyanide solution
Flow-control enters blender mixing in 0.5t/h respectively through respective liquid feed pump, controls mixer outlet temperature 30
DEG C, control Cyanogran. and liquid chlorine mol ratio to be 1：1.15；
（2）The feed liquid mixing is introduced tubular reactor, controls tubular type reactor pressure 0.8MPa, temperature will be reacted with recirculated water
Degree controls at 40 DEG C, reaction time 30s, sampling detection；
（3）After the completion of reaction, feed liquid enters Analytic Tower from the tail end of tubular reactor, the temperature control of Analytic Tower at 50 DEG C, through solution
Analyse, be dried to obtain pure chlorine dicyanogen body, conversion ratio reaches 99.55%.
Embodiment 2
（1）After intelligent flow meter accurate flow adjustment, liquid chlorine flow-control in 0.5t/h, 30% sodium cyanide solution
Flow-control enters blender mixing in 1.1t/h respectively through respective liquid feed pump, controls mixer outlet temperature 40
DEG C, control Cyanogran. and liquid chlorine mol ratio to be 1：1.045；
（2）The feed liquid mixing is introduced tubular reactor, controls tubular type reactor pressure 1.2MPa, temperature will be reacted with recirculated water
Degree controls at 45 DEG C, reaction time 50s, sampling detection；
（3）After the completion of reaction, feed liquid enters Analytic Tower from the tail end of tubular reactor, the temperature control of Analytic Tower at 60 DEG C, through solution
Analyse, be dried to obtain pure chlorine dicyanogen body, conversion ratio reaches 99.35%.
Claims (5)
1. a kind of method of use tubular reactor produced cyanogen chloride it is characterised in that：Including：By liquid chlorine and sodium cyanide solution
It is 1 by Cyanogran. and liquid chlorine mol ratio：0.9～1.2 ratio mixing, and control its temperature at 20～50 DEG C, then will mix
Liquid is passed through reaction in tubular reactor, controls tubular type reactor pressure 0.1～2.0MPa, reaction temperature controls at 20～60 DEG C,
Reaction time is 10～600s；
Feed liquid after the completion of reaction is entered Analytic Tower from the tail end of tubular reactor, the temperature control of Analytic Tower is 20～60
DEG C, through parsing, it is dried to obtain pure cyanogen chloride gas.
2. method according to claim 1 is it is characterised in that described sodium cyanide solution is 30% sodium cyanide solution,
Itself and liquid chlorine are respectively through liquid feed pump feeding, and after respective effusion meter accurate flow adjustment, enter blender and mix
Close, at control mixer outlet, feed temperature is at 20～50 DEG C.
3. method according to claim 1 is it is characterised in that control tubular type reactor pressure 0.4～1.5MPa.
4. method according to claim 1 is it is characterised in that control tubular type reactor pressure 0.6～1.0MPa.
5. method according to claim 1 is it is characterised in that reaction time is 20～300s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610780155.0A CN106395861A (en) | 2016-08-31 | 2016-08-31 | Method for producing cyanogen chloride by using tubular reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610780155.0A CN106395861A (en) | 2016-08-31 | 2016-08-31 | Method for producing cyanogen chloride by using tubular reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106395861A true CN106395861A (en) | 2017-02-15 |
Family
ID=58000220
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610780155.0A Pending CN106395861A (en) | 2016-08-31 | 2016-08-31 | Method for producing cyanogen chloride by using tubular reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106395861A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434253A (en) * | 2017-08-06 | 2017-12-05 | 河北诚信有限责任公司 | A kind of continuous production technology and its production system of high-quality cyanide solution |
| CN108622916A (en) * | 2018-07-04 | 2018-10-09 | 营口昌成化工科技有限公司 | A method of preparing cyanogen chloride |
| CN110902696A (en) * | 2019-08-28 | 2020-03-24 | 扬州天启新材料股份有限公司 | Preparation method of cyanogen chloride |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1525653A (en) * | 1975-05-12 | 1978-09-20 | Degussa | Process for the production of cyanogen chloride |
| CN101423230A (en) * | 2007-11-01 | 2009-05-06 | 埃沃尼克德古萨有限责任公司 | Process for preparing chlorocyan |
| CN101450808A (en) * | 2007-11-30 | 2009-06-10 | 江都市吴桥树脂厂 | Preparation method of cyanogen chloride |
| CN104925829A (en) * | 2015-06-03 | 2015-09-23 | 营创三征(营口)精细化工有限公司 | Chlorination reaction device and chlorination reaction technology for preparing cyanogen chloride |
-
2016
- 2016-08-31 CN CN201610780155.0A patent/CN106395861A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1525653A (en) * | 1975-05-12 | 1978-09-20 | Degussa | Process for the production of cyanogen chloride |
| CN101423230A (en) * | 2007-11-01 | 2009-05-06 | 埃沃尼克德古萨有限责任公司 | Process for preparing chlorocyan |
| CN101450808A (en) * | 2007-11-30 | 2009-06-10 | 江都市吴桥树脂厂 | Preparation method of cyanogen chloride |
| CN104925829A (en) * | 2015-06-03 | 2015-09-23 | 营创三征(营口)精细化工有限公司 | Chlorination reaction device and chlorination reaction technology for preparing cyanogen chloride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434253A (en) * | 2017-08-06 | 2017-12-05 | 河北诚信有限责任公司 | A kind of continuous production technology and its production system of high-quality cyanide solution |
| CN108622916A (en) * | 2018-07-04 | 2018-10-09 | 营口昌成化工科技有限公司 | A method of preparing cyanogen chloride |
| CN110902696A (en) * | 2019-08-28 | 2020-03-24 | 扬州天启新材料股份有限公司 | Preparation method of cyanogen chloride |
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Application publication date: 20170215 |
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