CN1424381A - Devices for continuously producing chlorinated paraffin - Google Patents

Devices for continuously producing chlorinated paraffin Download PDF

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Publication number
CN1424381A
CN1424381A CN 02148592 CN02148592A CN1424381A CN 1424381 A CN1424381 A CN 1424381A CN 02148592 CN02148592 CN 02148592 CN 02148592 A CN02148592 A CN 02148592A CN 1424381 A CN1424381 A CN 1424381A
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China
Prior art keywords
reactor
liquid phase
production apparatus
group
discharge port
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CN 02148592
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Chinese (zh)
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周南
韩陵陵
乐毅
赵云峰
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ZHENHAI ZHONGLI CHEMICAL INDUSTRY Co Ltd NINGBO CITY
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ZHENHAI ZHONGLI CHEMICAL INDUSTRY Co Ltd NINGBO CITY
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Priority to CN 02148592 priority Critical patent/CN1424381A/en
Publication of CN1424381A publication Critical patent/CN1424381A/en
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Abstract

An equipment for continuously chlorinating paraffin wax is composed of at least two reactors with gas phase inlet and outlet and liquid phase inlet and outlet. It features that all the reactors are divided into two groups, whose feeding and discharging are in parallel mode, and the liquid levels for the reactor in same group are sequentially decremented. Its advantages are high productivity and quality of product, and long service life.

Description

Continuous chloroparaffin production apparatus
Technical field
The present invention relates to produce in a kind of chemical industry the device of clorafin, especially a kind of technical field that adopts continuous production method to produce the clorafin device.
Background technology
The clorafin main application is the extender plasticizer that is used for polyvinyl chloride, and has certain fire retardation, also can be used as antithrombotics, tackifier, machining oil, paint stablizer and tanning agent.Along with high speed development of national economy, the continuous increase of plastics and plastics output, the range of application of clorafin also constantly enlarges.
Clorafin in last century the '30s begin suitability for industrialized production.The annual production of whole world clorafin at present has more than 50 ten thousand tons approximately.In mainly concentrating on, country such as American and Britain, moral, method, day.China is maximum clorafin producing country, about more than 20 ten thousand tons of throughput, about 120,000 tons of the throughput of the U.S..
According to investigations, up to the present no matter domestic be that preparation is hanged down the clorafin of chlorinity or high chlorine contents except that the technology of the photochemical catalysis serialization that Zhenhai Zhongli Chemical Industry Co., Ltd., Ningbo City had, more sophisticated relatively technology is thermal chlorination interrupter method production technique, this method is chemical plant, Shenyang Success in Experiment, She Ji 5m the earliest at home 3Enamel still adds the cervical part of esophagus gaseous phase section, with the pneumatic outer circulation refrigerative of graphite cooler thermal chlorination production technique.Some other factory also once went to inquire into serialization production with tower device, but all immature.
External production technique has bubble tower, spray tower, falling-film tower to realize multistage sectional continuous process, but suffer from all that equipment bulky complex, technical process are long, power consumption reaches drawbacks such as operation control is loaded down with trivial details greatly, and is unsatisfactory.Even Japan carbide company limited adopts 6m 3Enamel still, adopt the thermal chlorination batch production.Other external major company also adopts thermal chlorination to produce clorafin.
Zhenhai Zhongli Chemical Industry Co., Ltd., Ningbo City began to adopt the Zhejiang Provincial Chemical Engineering Research Inst technology to produce clorafin in 1996.Reaction unit is that three enamel stills and two groups of pipeline reactor series connection form flow process, and the gradient height between still and the still needs layered arrangement, and investment is big, and ability is little.This device designed capacity is 2500 tons/year, and through the production examination in 1 year, its actual capacity only was 1000 tons/year, be significantly less than design scale, and produce extremely instability, quality product is inferior, in the product very major part be unacceptable product, best product also only is salable product.
Many sharp chemical industry in 1997 are explored wax oil chlorating reaction characteristics through technical renovation, have invented " continous way is produced the device of clorafin ", and obtain national inventing patent (ZL981004570.7).The reactor of this device is a multi-step type cabin reactor.The successful operation of this device, make produce stablized, efficient and realized serialization.But this device also has its major defect, one, and strength problem: because manufacturing process and reactor design, the material of type cabin reactor is a glass reinforced plastic, because the uncertainty of glass reinforced plastic construction is calculated its intensity and is difficult to accurately; Moreover under reaction conditions, the osmosis aging and wax oil of glass reinforced plastic greatly descends the intensity of reaction unit, make device have potential safety hazard, and the decline of intensity easily causes device distortion to occur, phenomenons such as seepage, and the equipment distortion causes the Glass lamp casing collapse easily, influences ordinary production.Its two, reparation property is poor: wax oil is the releasing agent of glass reinforced plastic construction, contains some wax oils because the osmosis of wax oil makes in the body of reactor, this makes the glass reinforced plastic repairing again and original glass reinforced plastic be difficult to bonding.For above-mentioned reasons, the life-span of glass reinforced plastic type cabin reactor only is 2-3.Its three because the Chlorination tube mouth of glass reinforced plastic type cabin reactor, lamp sleeve opening are arranged in the side of equipment, changing logical chlorine valve and lamp sleeve pipe needs the material emptying in the equipment, very complicated; Its four, this device is inconvenient to overhaul.
Summary of the invention
Technical problem to be solved by this invention is that a kind of continuous chloroparaffin production apparatus low, safe and reliable, that maintenance is simple and the life-span is long of investing is provided at above-mentioned prior art present situation.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: this kind continuous chloroparaffin production apparatus, it comprises at least two reactors, each reactor is equipped with the gas-phase feed mouth, the gas phase discharge port, liquid phase feeding mouth and liquid phase discharge port, all reactors are divided at least two groups, parallel form is adopted in the turnover of liquid phase material between the group internal reaction still, and between group in the reactor liquid level of liquid phase material be little staged and successively decrease successively, liquid phase material flows into the low reactor group of liquid level position from the high reactor group of liquid level position successively with the series connection form, gaseous phase materials chlorine then enters each reactor with parallel form, and reaction end gas promptly imports same engine manifold after each reactor is discharged.Each reactor is independent, helps selecting for use the reactor of suitable material manufacturing, thereby guarantees the intensity of reactor, and such layout also helps maintenance and maintenance simultaneously.Moreover, above-mentioned material turnover form can guarantee the pressure basically identical in each reactor, thereby only to need realizing between group in the reactor liquid level of liquid phase material to be little staged successively decreases successively, liquid phase material can be from the high reactor group of liquid level position to the low reactor group of liquid level position with flow by gravity, help reducing cost of investment and running cost like this.From above-mentioned explanation, can learn, continuous chloroparaffin production apparatus of the present invention, can adopt the reactor more than two or two to constitute a reactor group, parallel form is adopted in the turnover of liquid phase material between the group internal reaction still, and the turnover employing of the liquid phase material form of connecting between this reactor group and other reactors or the reactor group.
All only contain a reactor in described each reactor group group, such design is a kind of preferred mode of the present invention, can reduce too loaded down with trivial details unit, is more convenient for actually operating.The number of reactor is advisable with 3~8.
The difference H of the liquid level of liquid phase material 0≤H≤1000mm within following ranges in the two adjacent groups reactor, low more H value helps reducing the requirement to the factory building height and the number of plies more, but also need satisfy suitable traffic requirement simultaneously.Find that through test its preferable scope is 50≤H≤200mm.
Described each reactor kettle top is provided with at least one catalysis socket, and the catalysis socket is equipped with a lamp sleeve pipe of vertically setting up, and in the lamp sleeve pipe light source is installed.Adopt light-catalysed advantage to be: temperature of reaction can hotter method reduce 30-35 ℃, and temperature of reaction is low, can make the color and luster of product be close to water white transparency.The number of catalysis socket can be done corresponding arrangement according to the size of reactor, is generally 2~4, and light source is evenly distributed in reactor.
The bottom that described liquid phase feeding mouth and liquid phase discharge port both can be arranged in the reactor kettle also can be arranged in the side of kettle, and gas-phase feed mouth, discharge port all are advisable with the top that is arranged in kettle.Liquid phase inlet and outlet piping between each group reaction still arranges it can is to go out that side is advanced the end or side goes out that the end is advanced or the end goes out that the end is advanced or side is advanced side and gone out.
Temperature is tending towards even in the reactor in order to make, the chlorinity that local superheating and wax oil do not occur is even, described each reactor is provided with liquid phase pump circulation discharge port and liquid phase pump circulation opening for feed, and between liquid phase pump circulation discharge port and liquid phase pump circulation opening for feed recycle pump and circulating line is installed.
Described each reactor all has and is used to the chuck that cools off or heat, heat so that when device is driven, reach temperature of reaction as early as possible by chuck, when ordinary production then by the chuck cooling to take away the heat that produces in the reaction process.For the throughput that makes device increases, take away the heat that produces in the reaction process, also can be on described liquid phase pump circulation pipeline mounting heat exchanger.Certainly, if the heat interchanging area of reacting kettle jacketing is enough, the interchanger in the forced circulation system can not installed yet.Same, if the heat interchanging area of the interchanger in the forced circulation system is enough, described each reactor is strap clamp cover not also.
Described each reactor is advisable to select enamel reaction still for use.Enamel reaction still makes that reaction unit is withstand voltage, heat resistance greatly improves, and equipment is not yielding, and the lamp sleeve pipe is difficult for breaking.Easy care, life-span are long, have more security than type cabin reactor.
Compared with prior art, continuous chloroparaffin production apparatus provided by the invention shows in the use of the Zhenhai, Ningbo City, Zhejiang Province sharp chemical industry of crowd company limited, although device of the present invention is to be combined by multiple devices, seem complicated, safeguard convenient more many than type cabin reactor.Because the Chlorination tube mouth of type cabin reactor, lamp sleeve opening are arranged in the side of equipment, changing logical chlorine valve and lamp sleeve pipe needs the material emptying in the equipment, very complicated; And the Chlorination tube mouth of apparatus of the present invention, lamp sleeve opening be all at the top, the material emptying of changing that valve, lamp sleeve pipe are extremely convenient in will equipment.The insufficient strength of type cabin reactor easily produces distortion again, and the equipment distortion easily causes glass bushing to break.Through post-installation review, chloroparaffin production apparatus of the present invention is compared with " continous way is produced the clorafin device " (type cabin reactor), invest lower slightly, production efficiency is slightly high, and quality product is good on an equal basis, but intensity is higher, conservative estimation device lifetime also will prolong 3~4 times, and the device good pressure-resistant performance, not yielding and seepage, maintenance is few.In a word, the former also has characteristics such as safe and reliable, that maintenance is simple, the life-span is long except that all superiority with latter.
Description of drawingsFig. 1 is the process flow sheet of the embodiment of the invention one; Fig. 2 is the process flow sheet of the embodiment of the invention two; Fig. 3 is the structural representation of reactor among Fig. 1 and Fig. 2.
Specific embodimentEmbodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one
As shown in figures 1 and 3, be a preferred embodiment of the present utility model.As shown in Figure 1, the described continuous chloroparaffin production apparatus of present embodiment is combined by five enamel reaction stills that have a chuck 1~5 and many supporting with it liquid phase forced circulation pumps 6, many interchanger 7 and the relevant supporting pipeline that is installed on the pump circulation pipeline.Five reactors are divided into five groups, promptly all only contain a reactor in each group group, and the mounting height of each reactor is little staged from 1 to No. five reactor 5 of a reactor successively decreases successively, and the height difference H between adjacent two reactors is 70mm.
As shown in Figure 3, the top of above-mentioned each reactor is provided with gas-phase feed mouth 8, gas phase discharge port 9, catalysis socket 10 and liquid phase pump circulation opening for feed 11, the bottom of reactor is provided with liquid phase pump circulation discharge port 12 and liquid phase discharge port 13, and the top, side of reactor is provided with liquid phase feeding mouth 14.In addition, also be provided with standby mouth 15 and visor etc. on the reactor.
Under the certain reaction condition, Witco 70 adds a reactor 1 through liquid phase feeding mouth 14, paraffin oil in reactor 1 with the chlorine reaction that feeds from top gas-phase feed mouth 8, for making gas distribution even, can be provided with gas distributor, the tail gas that reaction generates is discharged from reactor 1 a top gas phase discharge port 9, reacted paraffin oil flows into No. two reactors 2 from No. two reactor 2 lateral liquid phase feeding mouths 14 after flowing out from reactor 1 a bottom liquid phases discharge port 13 automatically, the chlorine that wax oil feeds with the top in No. two reactors 2 once more further reacts, and reaction end gas is discharged from No. two reactor 2 tops and compiled with tail gas that reactor 1 is discharged.Liquid phase material flows into reactor 1, No. two reactors 2, No. three reactors 3, No. four reactors 4 and No. five reactors 5 like this successively, in each reactor, carry out chlorination reaction with chlorine, the chloride of wax oil also progressively improved successively, and the clorafin that chlorinity meets the demands flows out from No. five reactors 5 at last.The reaction end gas of each reactor is discharged from the top and is imported engine manifold 16, enters exhaust treatment system again.As from the foregoing, liquid phase material is that automatically high reactor goes downstream and flows into the low reactor in position successively from the position, and promptly liquid phase material is by series system each reactor of flowing through successively from high to low.And gaseous phase materials is to enter each reactor simultaneously, and gas material pools together again after going out each reactor.Be that gaseous phase materials is by parallel way each reactor of flowing through.
In order to make each enamel reaction still liquid phase even, local superheating does not appear, each reactor all is provided with the liquid phase forced circulation system, it is by the liquid phase pump circulation discharge port 12 that is located at the reactor bottom, be located at the liquid phase pump circulation opening for feed 11 at top, and the recycle pump 6 and the circulating line that are installed between liquid phase pump circulation discharge port 12 and the liquid phase pump circulation opening for feed 11 are formed.For the throughput that improves reactor, the amount of shifting out that increases reaction heat, also on liquid phase pump circulation pipeline, interchanger 7 is installed, the material of interchanger 7 can be tetrafluoroethylene, enamel, glass and graphite etc.The effect of pump circulation is that to make liquidus temperature evenly reach the chlorinity of wax oil even, circulation ratio be circulation fluid per hour in internal circulating load and the reactor ratio of amount of liquid be 2-5 doubly.The material of pump can be that fluorine is moulded alloy, enamel etc.
Reaction heat take away by the water coolant in each reacting kettle jacketing and the liquid phase forced circulation system in interchanger 7 take away.If the heat interchanging area of reacting kettle jacketing is enough, the interchanger 7 in the liquid phase forced circulation system also can be installed.
For reaction also can be carried out at low temperatures, be provided with many catalysis sockets 10 at the reactor top, its number can be decided as the case may be, is provided with two catalysis sockets 10 in the present embodiment, is used for light-catalysed light source so that install.
Wax oil chlorination reaction in the entire reaction device all adopts photochemical catalysis, and temperature is controlled at 70-100 ℃, and pressure-controlling is at 0.01-0.05Mpa.Paraffin oil is 20-30 hour at the average waiting time of reactor assembly.Relatively seeing the following form of present embodiment continuous chloroparaffin production apparatus and other chloroparaffin production apparatus:
Sequence number Project Thermal chlorination The present embodiment device Glass reinforced plastic cabin formula reaction unit The Zhejiang Provincial Chemical Engineering Research Inst design apparatus
????1 The catalysis form Thermal chlorination Photochemical catalysis Photochemical catalysis Photochemical catalysis
????2 Production method Interrupter method Serialization Serialization Basic serialization
????3 Reaction times 40-60 hour 20-30 hour 20-30 hour 20-30 hour
????4 Energy consumption High Low Low High
????5 Operational condition Loaded down with trivial details Simple and easy steady Simple and easy steady Difficulty is big
????6 Quality product Unstable Excellent Excellent Generally
????7 Investment Generally Economize Economize Greatly
????8 Device lifetime Long Long Short Long
????9 Safeguard Easily Easily Difficult Easily
????10 Raw material consumption High Low Low Low
????11 Environmental protection Easily pollute Do not have leakage, pollute Small leakage, pollution are arranged Small leakage, pollution are arranged
????12 Throughput Low (120t/m3.) High (280t/m3.) High (240t/m3.) Low
????13 Floor space Greatly Little Little Greatly
????14 The factory building requirement Two layers Three layers Three layers At least four layers
????15 Security Generally High Generally Low
Embodiment two
As shown in Figures 2 and 3, be another preferred embodiment of the present utility model.As shown in Figure 2, the described continuous chloroparaffin production apparatus of present embodiment is also combined by five enamel reaction stills that have a chuck 1~5 and many supporting with it liquid phase forced circulation pumps 6, many interchanger 7 and the relevant supporting pipeline that is installed on the pump circulation pipeline.The difference of present embodiment and embodiment one is: five reactors are divided into four groups in the present embodiment, and wherein a reactor 1 and No. two reactors 2 constitute one group jointly, and other three reactors respectively become one group.The turnover of 2 groups of interior liquid phase materials of a reactor 1 and No. two reactors adopts the mounting height of parallel way and two stills consistent.

Claims (10)

1, a kind of continuous chloroparaffin production apparatus, it comprises at least two reactors, each reactor is equipped with gas-phase feed mouth (8), gas phase discharge port (9), liquid phase feeding mouth (14) and liquid phase discharge port (13), it is characterized in that all reactors are divided at least two groups, parallel form is adopted in the turnover of liquid phase material between the group internal reaction still, and between group in the reactor liquid level of liquid phase material be little staged and successively decrease successively, liquid phase material flows into the low reactor group of liquid level position from the high reactor group of liquid level position successively with the series connection form, gaseous phase materials then enters each reactor with parallel form, and reaction end gas promptly imports same engine manifold after each reactor is discharged.
2, continuous chloroparaffin production apparatus as claimed in claim 1 is characterized in that all only containing a reactor in described each reactor group group.
3, continuous chloroparaffin production apparatus as claimed in claim 1 or 2 is characterized in that difference H 0≤H≤1000mm within following ranges of the liquid level of liquid phase material in the two adjacent groups reactor.
4, continuous chloroparaffin production apparatus as claimed in claim 1 or 2, it is characterized in that described each reactor kettle top is provided with at least one catalysis socket (10), catalysis socket (10) is connected with a lamp sleeve pipe of vertically setting up, and in the lamp sleeve pipe light source is installed.
5, continuous chloroparaffin production apparatus as claimed in claim 1 or 2, it is characterized in that described liquid phase feeding mouth (14) is arranged in the side or the bottom of reactor kettle, described liquid phase discharge port (13) is arranged in the bottom or the side of kettle, and gas-phase feed mouth (8), gas phase discharge port (9) are arranged in the top of kettle.
6, continuous chloroparaffin production apparatus as claimed in claim 1 or 2, it is characterized in that liquid phase flow between each reactor group for from streamed, the liquid phase inlet and outlet piping between its each group reaction still arranges it can is to go out that side is advanced the end or side goes out that the end is advanced or the end goes out that the end is advanced or side is advanced side and gone out.
7, continuous chloroparaffin production apparatus as claimed in claim 1 or 2, it is characterized in that described each reactor is provided with liquid phase pump circulation discharge port (12) and liquid phase pump circulation opening for feed (11), and between liquid phase pump circulation discharge port (12) and liquid phase pump circulation opening for feed (11), recycle pump (6) and circulating line are installed.
8, continuous chloroparaffin production apparatus as claimed in claim 1 or 2, it is characterized in that described each reactor all have be used for the heating or the refrigerative chuck.
9, continuous chloroparaffin production apparatus as claimed in claim 1 or 2 is characterized in that described each reactor is an enamel reaction still.
10, continuous chloroparaffin production apparatus as claimed in claim 7 is characterized in that on the described liquid phase pump circulation pipeline interchanger (7) being installed.
CN 02148592 2002-12-18 2002-12-18 Devices for continuously producing chlorinated paraffin Pending CN1424381A (en)

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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100371425C (en) * 2006-04-03 2008-02-27 上海氯碱化工股份有限公司 Continuous production method of chlorinated paraffin
CN100371426C (en) * 2006-04-03 2008-02-27 上海氯碱化工股份有限公司 Continuous chloroparaffin production apparatus
CN102145251A (en) * 2011-01-06 2011-08-10 鲁西化工集团股份有限公司氯碱化工分公司 Dechloridation device and process in chlorinated paraffin production process
CN103060000A (en) * 2013-01-05 2013-04-24 沁阳市海世鸿工贸有限责任公司 Chlorinated paraffin production equipment and method
CN103642525A (en) * 2013-11-22 2014-03-19 大连隆星新材料有限公司 Reaction tower for preparing chlorinated paraffin by photocatalysis
CN103666562A (en) * 2013-11-13 2014-03-26 吕德斌 Unpowered circulating chlorinated paraffin reaction device with single kettle and reactors
CN103849433A (en) * 2013-03-26 2014-06-11 洛阳欧克迈自控工程有限公司 Automatic production technology of chlorinated paraffin
CN103923701A (en) * 2013-11-22 2014-07-16 大连隆星新材料有限公司 Multistage jacketed chlorinated paraffin reaction tower
CN103965963A (en) * 2014-03-24 2014-08-06 辛集市三金化工有限公司 Chlorinated paraffin production equipment and automatic control system
CN104673388A (en) * 2013-11-28 2015-06-03 大连隆星新材料有限公司 Chlorinated paraffin device
CN104862008A (en) * 2015-05-28 2015-08-26 沧州兴达化工有限责任公司 Continuous production system of environment-friendly rubber softener
CN106892812A (en) * 2017-03-09 2017-06-27 兖矿鲁南化工有限公司 The system and technique of a kind of synthesizing acetic anhydride by carbonyl under low pressure
CN110420611A (en) * 2019-09-06 2019-11-08 丹阳市助剂化工厂有限公司 A kind of chlorination tank producing chlorinated paraffin
CN111926178A (en) * 2020-08-11 2020-11-13 昆明理工大学 Device and method for cracking organic matters in zinc sulfate solution

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100371426C (en) * 2006-04-03 2008-02-27 上海氯碱化工股份有限公司 Continuous chloroparaffin production apparatus
CN100371425C (en) * 2006-04-03 2008-02-27 上海氯碱化工股份有限公司 Continuous production method of chlorinated paraffin
CN102145251A (en) * 2011-01-06 2011-08-10 鲁西化工集团股份有限公司氯碱化工分公司 Dechloridation device and process in chlorinated paraffin production process
CN103060000A (en) * 2013-01-05 2013-04-24 沁阳市海世鸿工贸有限责任公司 Chlorinated paraffin production equipment and method
CN103849433A (en) * 2013-03-26 2014-06-11 洛阳欧克迈自控工程有限公司 Automatic production technology of chlorinated paraffin
CN103666562B (en) * 2013-11-13 2015-11-25 吕德斌 Unpowered circulation single still multiple reactor clorafin reaction unit
CN103666562A (en) * 2013-11-13 2014-03-26 吕德斌 Unpowered circulating chlorinated paraffin reaction device with single kettle and reactors
CN103642525A (en) * 2013-11-22 2014-03-19 大连隆星新材料有限公司 Reaction tower for preparing chlorinated paraffin by photocatalysis
CN103642525B (en) * 2013-11-22 2015-08-26 大连隆星新材料有限公司 For the reaction tower of Preparation of Chloroparaffin by Photo-catalytic Method
CN103923701A (en) * 2013-11-22 2014-07-16 大连隆星新材料有限公司 Multistage jacketed chlorinated paraffin reaction tower
CN104673388A (en) * 2013-11-28 2015-06-03 大连隆星新材料有限公司 Chlorinated paraffin device
CN103965963A (en) * 2014-03-24 2014-08-06 辛集市三金化工有限公司 Chlorinated paraffin production equipment and automatic control system
CN104862008A (en) * 2015-05-28 2015-08-26 沧州兴达化工有限责任公司 Continuous production system of environment-friendly rubber softener
CN106892812A (en) * 2017-03-09 2017-06-27 兖矿鲁南化工有限公司 The system and technique of a kind of synthesizing acetic anhydride by carbonyl under low pressure
CN106892812B (en) * 2017-03-09 2020-02-28 兖矿鲁南化工有限公司 Process for synthesizing acetic anhydride by low-pressure carbonyl
CN110420611A (en) * 2019-09-06 2019-11-08 丹阳市助剂化工厂有限公司 A kind of chlorination tank producing chlorinated paraffin
CN111926178A (en) * 2020-08-11 2020-11-13 昆明理工大学 Device and method for cracking organic matters in zinc sulfate solution

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