CN105541673B - A kind of method of duct type continuous production CLT acid itrated compound - Google Patents
A kind of method of duct type continuous production CLT acid itrated compound Download PDFInfo
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- CN105541673B CN105541673B CN201610024031.XA CN201610024031A CN105541673B CN 105541673 B CN105541673 B CN 105541673B CN 201610024031 A CN201610024031 A CN 201610024031A CN 105541673 B CN105541673 B CN 105541673B
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- 0 C*c1cc(*)ccc1* Chemical compound C*c1cc(*)ccc1* 0.000 description 4
- CDPWHWNALGTROU-BQYQJAHWSA-N CCC/C(/C)=C(\CCS(O)(=O)=O)/Cl Chemical compound CCC/C(/C)=C(\CCS(O)(=O)=O)/Cl CDPWHWNALGTROU-BQYQJAHWSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method of duct type continuous production CLT acid itrated compound, including：Step (1)：Toluene and sulfuric acid, which are passed to, carries out sulfonating reaction in sulfonation pipeline reactor；Step (2)：The sulfonating reaction liquid that step (1) is obtained continuously passes to chlorine and chlorination reaction is carried out in chlorination pipeline reactor；Step (3)：The chlorination reaction liquid that step (2) is obtained continuously passes in nitrification pipeline reactor with nitric acid and carries out nitration reaction, obtains CLT acid itrated compound.In the present invention, course of reaction to intermediate without carrying out purification process, and simple to operate, reaction efficiency is high, and purpose product selectivity is high.
Description
Technical field
The present invention relates to the synthesis field of organic pigment intermediate, more particularly to a kind of duct type continuous production CLT acid
The method of itrated compound.
Background technology
CLT acid (CLT acid) is also known as C acid, and chemical name is the chloro- 3- amino toluenes -4- sulfonic acid of 6-, and relative molecular weight is
221.CLT acid is white or reddish Solid powder, substantially nontoxic, is slightly soluble in water, is soluble in ammoniacal liquor and alkali lye, is that synthesis is red
The important intermediate of organic pigment.The bright red LC of everbright red toner C and rubber synthesized by CLT acid is mainly used in ink, rubber and text
The coloring of articles for use is taught, is lasting, indispensable high-grade organic red pigment in the world.
At present, CLT acid synthetic method both domestic and external is substantially toluene sulfonation method, synthetic route square formula 1：
As shown in equation 1, the sulfonated CLT acid sulfonated bodies, CLT acid sulfonated bodies chlorination of obtaining of toluene obtains CLT acid chlorination
Thing, CLT acid chloride nitrification obtain CLT acid itrated compound, and CLT acid itrated compound obtains CLT acid finished product through reduction.This method raw material comes
Source is wide, simple to operate, production cost is low.
Conventional sulfonation reactor has autoclave, pot group type, membrane type, injecting type etc. at present.Wherein, batch (-type) autoclave and tank group
The alternate contact area of formula sulfonation reactor is small, and mass-and heat-transfer effect is poor, low production efficiency；Film sulfonation reactor is complicated,
Processing, manufacture and the installation accuracy of equipment require all higher, and investment cost is big, and operating flexibility is small, and driving and parking is inconvenient, and heat exchange
Limited area, the reaction for SO 3 sulfonated toluene easily produces hot-spot, can reduce the selectivity of product, be unfavorable for
The progress of sulfonating reaction.
A kind of Publication No. CN1566083A manufacture method of naphthalene sulfonic acids of Chinese patent literature, naphthalene continuous and quantitative is pumped into
In membrane type or shell and tube reactor, while feeding contains SO in proportion3The sulfonating agent of gas, naphthalene is flowed down along reactor wall in membranaceous,
With SO3Gas is contacted, and moment reacts, and obtains the reaction product based on α-naphthalenesulfonicacid, by reaction product continuous conveying extremely
Aging device carries out isomerization, finally gives the naphthalene sulfonic acids product using beta-naphthalenesulfonic-acid as main component.This method uses sulfur trioxide
As sulfonating agent, reaction is violent, and heat is difficult to distribute, and was easily caused sulfonation, color and luster deterioration, charing and explosive oxidation etc. and lacks
Point.
In the prior art, CLT acid and its intermediate are prepared by batch tank mode more, it is cumbersome, purpose product
Poor selectivity, low production efficiency.
The content of the invention
To solve many defects of existing CLT acid synthetic method, the invention provides a kind of duct type continuous production CLT
The method of acid and its intermediate, compared with traditional batch reactor, consersion unit small volume, reaction stability be good,
Product selectivity is high.
To achieve the above object, the invention provides following technical scheme：
A kind of method of duct type continuous production CLT acid itrated compound, comprises the following steps：
Step (1)：Toluene and sulfuric acid, which are passed to, carries out sulfonating reaction in sulfonation pipeline reactor；
Step (2)：The sulfonating reaction liquid that step (1) is obtained continuously passes to chlorine and chlorination is carried out in chlorination pipeline reactor
Reaction；
Step (3)：The chlorination reaction liquid that step (2) is obtained continuously passes in nitrification pipeline reactor with nitric acid and carries out nitre
Change reaction, obtain CLT acid itrated compound.
Compared with existing batch tank reaction method, course of reaction controllability of the invention is good, purpose product selectivity is high；
Course of reaction effectively improves production efficiency without being purified to intermediate；In addition, can also reduce the dirt that toluene volatilizees to environment
Dye.
Described sulfonation pipeline reactor preferred pipeline formula liquid liquid static mixer.More preferably SK types duct type liquid
Liquid static mixer and/or SV type duct type liquid liquid static mixers.
In step (1), sulfonation pipeline reactor is first preheated to 90 DEG C -100 DEG C with steam；Then be pumped into respectively sulfuric acid and
Toluene.Charging carries out sulfonating reaction in the sulfonating reaction pipeline, and sulfonating reaction is produced in time by sulfonating reaction pipe outlet
Liquid, described sulfonating reaction liquid is the sulfuric acid solution of CLT acid sulfonated bodies.
The reaction equation square formula 2 of step (1)：
The mass percent concentration of described sulfuric acid is more than 98%, before sulfonation pipeline reactor is entered, is first preheated to 90-
100℃。
In step (1), the charged material weight ratio of toluene and sulfuric acid is 1:2~3.The charged material weight is than that can ensure the complete of toluene
Full response, it is to avoid unreacted toluene participates in the reaction such as follow-up chlorination, nitrification.
Preferably, the charged material weight ratio of toluene and sulfuric acid is 1:2.5.
The feed rate of sulfuric acid is preferably 200-300kg/h.
In step (1), the temperature of sulfonating reaction is 100~130 DEG C.Sulfonation pipe reaction is regulated and controled using temperature automatically controlled equipment
Temperature in device.
In course of reaction, continuous reaction state is monitored by HPLC, is a sampling period, the sample taken per 1-2h
Product are the reaction solution in sulfonation pipeline reactor exit.If the content of toluene is more than 1% in samples taken, suspend sample introduction, lead to
Connecting method extension sulfonation pipeline reactor is crossed, so as to extend reaction time (residence time in reactor), until toluene
Content is less than 1%.
Preferably, the duct length of described sulfonation pipeline reactor is 80-150m.More preferably 100m.
The touch opportunity of toluene and sulfuric acid is added using the pipe type continuously mode of production, alternate contact area is improved,
So as to improve sulfonating reaction efficiency；Reaction product can be transferred out of reactor in time, help to reduce the water that production process is produced
Influence to sulfonating reaction, reduces by-products content.Analyzed by HPLC, in sulfonating reaction liquid, p-methyl benzenesulfonic acid (CLT
Sour sulfonated bodies) content >=98% (area normalization method), the content of other by-products such as ortho position and meta substituent is ≤1.0%.
In sulfonating reaction liquid, the content of sulfuric acid solution is more than 60wt%.Without carrying out purification process to sulfonating reaction liquid, directly
Scoop out with the chlorination reaction to step (2).
The reaction equation square formula 3 of step (2).
The temperature of sulfonating reaction liquid is higher, before chlorination reaction, and sulfonating reaction liquid temperature degree first is down into 70-80 DEG C.To improve
The utilization rate of energy, by medium circulation to the chuck of chlorination pipeline reactor for cooling down sulfonating reaction liquid, for by chlorination pipe
Road reactor pre-heating temperature elevation is to 70-80 DEG C.
Preferably, described chlorination pipeline reactor is duct type gas-liquid static mixer.
In step (2), material in respective measuring pump pump to chlorination pipeline reactor by chlorination reaction is carried out, as excellent
Choosing, 1-1.3 times that adds the CLT acid sulfonated bodies that mole is sulfonating reaction liquid of chlorine.It that is to say, in step (2), chlorine
Add 1-1.3 times of mole equivalent to the toluene molar amount that step (1) is added.
Chlorination reaction temperature is 70-80 DEG C.Pass through temperature automatically controlled equipment regulating and controlling temperature.In process of production, HPLC is analyzed
The reaction solution of chlorination pipeline reactor tail end, monitors response situation.If in samples taken, the chromatographic content of p-methyl benzenesulfonic acid is more than
1%, suspend sample introduction, chlorination pipeline reactor is extended by connecting method, so as to extend the reaction time, until right in middle control sample
Toluenesulfonic acid content is less than 1%.
Preferably, the duct length of described chlorination pipeline reactor is 80-150m.
After continuous chlorination production terminates, HPLC analyses are carried out to chlorination reaction liquid and are known, the chloro- 4- toluene sulfonic acides (CLT of 3-
Sour chloride) content >=95%, other by-product chloride chromatogram total content≤5%；The selectivity of the chloro- 4- toluene sulfonic acides of 3-
Apparently higher than state of the art.
The content of CLT acid chloride in the chlorination reaction liquid that step (2) is obtained is very high, and also has to nitration reaction tool
There is the sulfuric acid (being introduced by step (1)) of catalytic action, the synthesis of CLT acid itrated compound can be directly applied to without purifying.
The equation square formula 4 of nitration reaction：
The model for the nitrification pipeline reactor that step (3) is used is as step (1), preferred pipeline formula liquid liquid static mixing
Device, also can adjust pipe according to the middle control result of raw material in the reaction solution of nitration reaction (the predominantly chloro- 4- toluene sulfonic acides of 3-)
Road length, so operation can improve nitration reaction efficiency, reduce accessory substance.
Preferably, in step (3), the duct length of described nitrification pipeline reactor is 80-150m.
Preferably, nitrification pipeline reactor is SK type duct type liquid liquid static mixers and/or SV type duct type liquid liquid
Static mixer.
Before nitration reaction, nitrification pipeline reactor is preheated to 65-75 DEG C.In actual production process, step (2) can be used
Chlorination reactor chuck in media preheating step (3) nitrification pipeline reactor.
During nitration reaction, the content that many nitros replace accessory substance will not be increased because of the increase of nitric acid inventory, but
Excessive nitric acid can produce wastes, preferably, nitric acid adds CLT acid chloride mole of the mole for chlorination reaction liquid
1-1.3 times.It that is to say, the mole that adds of the nitric acid of step (3) is 1-1.3 times that step (1) toluene adds mole.
Nitration reaction temperature is 70-80 DEG C.It is preferred that 70-75 DEG C.Temperature adjusting is carried out by temperature automatically controlled equipment.Middle control is anti-
At once, it is a sampling period per 1-2h, takes the reaction solution in pipeline reactor exit to carry out 3- in HPLC analyses, sample
It is qualified that the content of chloro- 4- toluene sulfonic acides, which is less than 1%,；If below standard, suspend sample introduction, pass through connecting method extension nitrification pipeline
Reactor, so as to extend the reaction time, until middle control detection is qualified.
Step (3) continuous production terminates, and the 2- nitro-4-methyl -5- chlorobenzenesulfonic acids content in nitration reaction liquid >=
90%th, other by-product≤10%.
Contain sulfuric acid and nitric acid in obtained CLT itrated compounds, without purification process, nitre is directly carried out under the catalysis of iron
Base reduction reaction, is made CLT acid.
Present invention also offers a kind of pipeline continuous production system of CLT acid itrated compound：Including the sulfonation being sequentially connected in series
Pipeline reactor, chlorination pipeline reactor and nitrification pipeline reactor；
Also include the CLT acid sulfonated bodies storage tank being connected between sulfonation pipeline reactor and chlorination pipeline reactor；Series connection
CLT chloride storage tanks between chlorination pipeline reactor and nitrification pipeline reactor；Nitrify the afterbody outlet of pipeline reactor
It is connected with CLT acid itrated compound reservoir inlet；
The sulfonation pipeline reactor is provided with toluene entrance and sulfuric acid entrance；Toluene tank is exported and sulfuric acid storage tank outlet point
It is not connected by measuring pump with respective entrance.
Measuring pump is provided between the connecting line of CLT acid sulfonated bodies storage tank and chlorination pipeline reactor；The chlorination pipe
Road reactor is additionally provided with chlorine inlet.
Measuring pump is provided between CLT chlorides storage tank and the connecting line for nitrifying pipeline reactor；The nitrification chlorination
Pipeline reactor is additionally provided with nitric acid entrance, and nitric acid storage tank is connected by measuring pump and nitric acid entrance.
Compared with prior art, beneficial effects of the present invention are：
Duct type serialization CLT acid sulfonated bodies, CLT acid chloride, CLT acid itrated compound are carried out using pipeline reactor
Production, course of reaction to intermediate without carrying out purification process, and simple to operate, reaction efficiency is high, and purpose product selectivity is high.
Embodiment
A kind of pipeline continuous production system of CLT acid itrated compound：Sulfonation duct type liquid liquid including being sequentially connected in series is static
Blender (SK types), chlorination duct type gas-liquid static mixer and nitrification duct type liquid liquid static mixer (SK types)；
Also include being connected between sulfonation duct type liquid liquid static mixer and chlorination duct type gas-liquid static mixer
CLT acid sulfonated bodies storage tank；It is connected between chlorination duct type gas-liquid static mixer and nitrification duct type liquid liquid static mixer
CLT chloride storage tanks；The afterbody outlet of nitrification duct type liquid liquid static mixer is connected with CLT acid itrated compound reservoir inlet；
The sulfonation duct type liquid liquid static mixer is provided with toluene entrance and sulfuric acid entrance；Toluene tank is exported and sulfuric acid
Outlet is connected by measuring pump with respective entrance respectively.
Measuring pump is provided between the connecting line of CLT acid sulfonated bodies storage tank and chlorination duct type gas-liquid static mixer；
The chlorination duct type gas-liquid static mixer is additionally provided with chlorine inlet.
Measuring pump is provided between CLT chlorides storage tank and the connecting line for nitrifying duct type liquid liquid static mixer；Institute
State nitrification duct type gas-liquid static mixer and be additionally provided with nitric acid entrance, nitric acid storage tank is connected by measuring pump and nitric acid entrance.
Embodiment 1
Step (1)：The synthesis of CLT acid sulfonated bodies：
To caliber DN10 sulfonation pipeline reactor (sulfonation duct type liquid liquid static mixer, SK types, length is 100m)
Chuck in be passed through steam, sulfonation pipeline reactor is preheated to 100 DEG C, steam off after the completion of preheating.Open 98% sulfuric acid
Material inlet valve, 98% sulfuric acid for being pre-heated to 100 DEG C is squeezed into reactor by measuring pump, controls 98% vitriolic acid flux to be
250kg/ hours；Toluene feed valve is opened simultaneously, is squeezed into normal temperature toluene in reactor by measuring pump, controls toluene flux
For 100kg/ hours.Continuous sample introduction material reacts in reactor inside holding, and temperature is 120-125 DEG C.
During continuous sulfonating reaction, continuous reaction state is monitored by HPLC, is a sampling period per 1-2h,
The sample taken is the reaction solution in sulfonation pipeline reactor exit.Specific experiment data are shown in Table 1：
Table 1
React the sulfonating reaction liquid completed and storage in CLT acid sulfonated bodies storage tank is entered by reactor outlet, be prepared to enter into down
One process.Sulfonating reaction liquid in HPLC analysis CLT acid sulfonated bodies storage tanks, wherein, p-methyl benzenesulfonic acid (CLT acid sulfonated bodies)
Chromatographic content is 99.3%, and maximum single impurity content is less than 0.4%.
Step (2)：The synthesis of CLT acid chloride：
Cooling medium is passed through into the chuck of CLT acid sulfonated bodies storage tank, material is cooled to 70 DEG C, then draws the medium
It is in the chuck for being directed at chlorination pipeline reactor (chlorination duct type gas-liquid static mixer, length is 100m), the reactor is pre-
Heat is to 70 DEG C.The caliber DN25 of chlorination pipeline reactor, length is 100m.
After the completion of the preheating of chlorination pipeline reactor, sulfonating reaction liquid is squeezed into chlorination pipeline reactor, sulfonating reaction liquid
Flow is 1000kg/ hours；Chlorine feed valve is opened simultaneously, and the speed by 320kg/ of flow hour is passed through in reactor,
By temperature in automatic temperature control system control chlorination pipeline reactor at 75-80 DEG C.Charging carries out serialization chlorination reaction, reaction
During, continuous reaction state is monitored by HPLC, is a sampling period per 1-2h, the sample taken is sulfonation pipeline
The reaction solution of reactor exit.Specific experiment data are shown in Table 2：
Table 2
React the chlorination reaction liquid completed and storage in CLT acid chloride storage tank is entered by the outlet of chlorination pipeline reactor, it is right
CLT acid chloride composition in storage tank carries out HPLC analyses, wherein, the chromatographic content of the chloro- 4- toluene sulfonic acides of 3- is 95.2%.
Without purification process, next process is directly entered.
Step (3)：CLT acid itrated compound is continuously synthesizing to；
(duct type liquid liquid static mixer, SK types are nitrified, length is to caliber for DN40 nitrification pipeline reactor
The medium of the reactor jacket of steam or step (2) is passed through in chuck 100m), by nitrification pipeline reactor pre-heating temperature elevation to 65
℃.Chlorination reaction liquid material inlet valve is opened, by measuring pump by CLT acid chloride pump to duct type liquid liquid static mixer,
The flow for controlling chlorination reaction liquid is 1500kg/ hours；98% nitric acid material inlet valve is opened simultaneously, nitric acid is pumped into, and controls nitric acid
Flow was at 300kg/ hours；By temperature in automatic temperature control system control pipeline formula liquid liquid static mixer at 70-75 DEG C, charging
Carry out serialization nitration reaction.During nitration reaction, by controlling reaction process in HPLC, serialization is monitored by HPLC anti-
State is answered, is a sampling period per 1-2h, the sample taken is the reaction solution in sulfonation pipeline reactor exit.In HPLC
Control result as shown in table 3：
Table 3
The sulfuric acid solution for reacting the CLT acid itrated compound mixture completed is entered by duct type liquid liquid static mixer outlet
Stored in CLT acid itrated compound storage tank, be prepared to enter into next process.
Iron is added into obtained CLT acid itrated compound, CLT acid is made in reduction, and preparation method is with reference to existing conventional method.
Comparative example 1：
The sulfuric acid of 25kg 98% and 10kg toluene are added into 50L reactor；Reacted at 120-125 DEG C.Controlled in HPLC
Reaction, once, specific experiment data are shown in Table 4 for sampling in every 2 hours：
Table 4
Embodiment 1 is compared with comparative example 1, the toluene conversion of embodiment 1 and the content of p-methyl benzenesulfonic acid comprehensively better than pair
Ratio 1.
Comparative example 2
Compared with embodiment 1, difference is, carry out the reaction of step (2) using reactor, the ingredient proportion of material and anti-
Answer temperature and time constant.
Experimental data is controlled in HPLC and is shown in Table 5：
Table 5
As shown in Table 5, lower using the chloro- 4- toluene sulfonic acides yields of 3- of the autoclave mode of production, by-product content is higher.
Comparative example 3
Compared with embodiment 1, difference is, carry out the reaction of step (3) using reactor, the ingredient proportion of material and anti-
Answer temperature and time constant.
Experimental data is controlled in HPLC and is shown in Table 6：
Table 6
Comparative example 3 is compared with embodiment 1, and the conversion ratio of the chloro- 4- toluene sulfonic acides of 3- is low, and is reacted to 6h and be substantially transitioned to
Accessory substance, by-products content is high, the poor selectivity of target product.
Claims (1)
1. a kind of method of duct type continuous production CLT acid itrated compound, it is characterised in that comprise the following steps：
Step (1)：Steam is passed through into the chuck of sulfonation pipeline reactor, sulfonation pipeline reactor is preheated to 100 DEG C, preheating
After the completion of steam off；98% sulfuric acid material inlet valve is opened, 98% sulfuric acid for being pre-heated to 100 DEG C is squeezed into instead by measuring pump
Answer in device, it is 250kg/ hours to control 98% vitriolic acid flux；Toluene feed valve is opened simultaneously, by measuring pump by normal temperature toluene
Squeeze into reactor, it is 100kg/ hours to control toluene flux；Continuous sample introduction material reacts in reactor inside holding, and temperature is
120-125 DEG C, during continuous sulfonating reaction, continuous reaction state is monitored by HPLC, is a sampling week per 1-2h
Phase, the sample taken is the reaction solution in sulfonation pipeline reactor exit；The sulfonating reaction liquid that reaction is completed is gone out by reactor
Mouth, which enters in CLT acid sulfonated bodies storage tank, to be stored, and is prepared to enter into next process；
Described sulfonation pipeline reactor is the SK type liquid liquid static mixers that caliber DN10, length are 100m；
Step (2)：Cooling medium is passed through into the chuck of CLT acid sulfonated bodies storage tank, material is cooled to 70 DEG C, then this is situated between
Matter is guided to the chuck of chlorination pipeline reactor, and the reactor is preheated into 70 DEG C；After the completion of the preheating of chlorination pipeline reactor,
Sulfonating reaction liquid is squeezed into chlorination pipeline reactor, sulfonating reaction flow quantity is 1000kg/ hours；Chlorine feed is opened simultaneously
Valve, the speed by 320kg/ of flow hour is passed through in reactor, is passed through automatic temperature control system and is controlled chlorination pipeline reactor
Interior temperature is at 75-80 DEG C；
In course of reaction, continuous reaction state is monitored by HPLC, is a sampling period per 1-2h, the sample taken is
The reaction solution in chlorination pipeline reactor exit；React the chlorination reaction liquid completed and CLT is entered by the outlet of chlorination pipeline reactor
Stored in sour chloride storage tank, without purification process, be directly entered next process；
Described chlorination pipeline reactor is the gas-liquid static mixer that caliber DN25, length are 100m；
Step (3)：The medium of the reactor jacket of steam or step (2) is passed through into the chuck of nitrification pipeline reactor, by nitre
Change pipeline reactor pre-heating temperature elevation to 65 DEG C, open chlorination reaction liquid material inlet valve, by measuring pump by CLT acid chloride pump extremely
In duct type liquid liquid static mixer, the flow for controlling chlorination reaction liquid is 1500kg/ hours；The charging of 98% nitric acid is opened simultaneously
Valve, is pumped into nitric acid, control nitric acid flow was at 300kg/ hours；Pass through temperature in automatic temperature control system control nitrification pipeline reactor
Degree is at 70-75 DEG C, and charging carries out serialization nitration reaction and obtains CLT itrated compounds；
During nitration reaction, by controlling reaction process in HPLC, continuous reaction state is monitored by HPLC, is per 1-2h
One sampling period, the sample taken is the reaction solution in nitrification pipeline reactor exit；
Described nitrification pipeline reactor is the liquid liquid static mixer that caliber DN40, length are 100m.
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