CN101766980A - Reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and synthesis process - Google Patents
Reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and synthesis process Download PDFInfo
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- CN101766980A CN101766980A CN200910256092A CN200910256092A CN101766980A CN 101766980 A CN101766980 A CN 101766980A CN 200910256092 A CN200910256092 A CN 200910256092A CN 200910256092 A CN200910256092 A CN 200910256092A CN 101766980 A CN101766980 A CN 101766980A
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Abstract
The invention relates to a reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and a synthesis process; the reactor is characterized in that: the reactor is mainly composed of a central cooling pipe, a reaction pipe filled with fillers and an outer cooling pipe; continuous synthesis of the tetrabromoethane is realized by continuous countercurrent contact reaction of the bromine and the acetylene in the reaction pipe, so as to improve the production efficiency; by adjusting the temperature and flow rate of the cooling water in the inner and outer cooling pipes, the addition reaction temperature can be controlled, the problems of safety and more by-products are solved owning to overhigh reaction temperature; by adopting the reactor and the synthesis process, the explosive mixture of acetylene and air is prevented from being formed in the reaction process, so as to improve the reaction safety.
Description
Technical field
The present invention relates to tetrabromoethane, particularly a kind ofly be used for bromine and acetylene gas carries out reactor and the synthesis technique that addition reaction prepares tetrabromoethane.
Background technology
1,1,2, the 2-tetrabromoethane is white or light yellow strong refractivity liquid, has the iodoform smell.Miscible, water insoluble with ethanol, ether, chloroform, aniline, glacial acetic acid.0 ℃ of fusing point.243.5 ℃ of boiling points, 151 ℃ (7.2kPa), 114 ℃ (0.267kPa).Relative density 2.9656 (20/4 ℃), refractive index 1.638.Illumination and can decompose its colour changed into yellow when being heated.Catabolite is the carbonyl bromide steam of severe toxicity when being higher than 190 ℃.Tetrabromoethane is a kind of important chemical auxiliary agent, uses in raw material polyester (PTA) production technology at terylene, changes into the co-catalyst of terephthalic acid (TPA) process as xylene oxygen; In staple fibre, plastic products such as polystyrene foamed plastics, be used as fire retardant; In trimellitic acid is produced, use and be catalyst; Also as the flotation fluid that separates rubble, the solvent of dyestuff intermediate, grease and wax is used for the mensuration of ore proportion and index of refraction, is used for synthetic pesticide, microscope instrument cleaning agent or the like.
Tetrabromoethane is to be raw material with acetylene, obtains through bromination, and the technological process of production is as follows:
Raw material → synthetic → neutralization → distillation → product
Acetylene gas is generated in acetylene generator by calcium carbide, after purification, drying, enters the reaction of reactor and bromine and obtains the tetrabromoethane crude product.The tetrabromoethane crude product through alkali cleaning, washing to remove acidic materials and water-soluble substances such as HBr, then by the rectified purified tetrabromoethane product that obtains.At present, bromine and acetylene mainly are batch process by the synthesis technique that addition reaction generates the tetrabromoethane crude product, and building-up process is mainly carried out in reactor.Utilize vacuum that a certain amount of bromine is pumped in the reactor earlier, acetylene gas is directly fed begin reaction in the still in the bromine then, generate the tetrabromoethane crude product.
But there is following problem in above-mentioned synthesis technique:
(1) after utilizing vacuum that bromine is added reactor, reactor is full of air, and the acetylene gas of Tong Ruing may mix the formation explosive mixture with the interior air of still subsequently.The aerial explosion limit of acetylene is 3%-81% (volume fraction), and acetylene and air form the compositing range of explosive mixture greater than other hydrocarbons.Therefore, there is potential safety hazard in this technical process, causes security incident easily.Though taked multiple measure, effect is undesirable.(2) addition reaction of bromine and acetylene is exothermic reaction, can emit a large amount of heats in the course of reaction, thereby makes temperature of reaction system raise.Temperature of reaction system is too high, and the bromine volatility is increased, and causes the bromine amount by the tail gas loss to increase.Simultaneously, too high temperature can increase the explosive mixture moral that acetylene and air form and fires possibility.Too high reaction temperature also can increase the probability that generates side reaction product, reduces product yield and product quality.(3) reactor that adopts at present can only carry out the synthetic production of batch (-type), can't produce continuously, influences the raising of production efficiency and productive rate, also causes the waste of raw material acetylene gas.
Summary of the invention
For solving the problem that exists in the synthesis technique, particularly synthesis reactor can't be produced continuously, form acetylene and air easily and form explosive mixture, exothermic heat of reaction can't in time be removed easily to problems such as reaction exert an influence, the invention provides a kind of reactor that bromine and acetylene addition reaction prepare tetrabromoethane that is used for, its objective is: can realize the continuous addition reaction of bromine and acetylene gas, enhance productivity and productive rate, improve the utilization rate of raw material acetylene gas; In time remove exothermic heat of reaction, avoid too high safety problem of bringing of temperature and the too much problem of accessory substance; Avoid forming the explosive mixture of acetylene and air, improve reaction safety.
The invention main points
A kind ofly be used for the reactor that bromine and acetylene addition reaction prepare tetrabromoethane, critical piece comprises the reaction tube (D) of center cooling tube (F), interior filling material, outer cooling tube (C), appeal three critical pieces and distribute successively from inside to outside, be combined as reactor body.
Described center cooling tube is one to have the straight type cooling tube of coolant inlet (G), coolant outlet (K), closed at both ends.Center cooling tube length equates that with tube length of reaction tube diameter is 1/3 of a reaction tube diameter.
Described reaction tube (D) is one to have the reaction tube of bromine charging aperture (I), acetylene gas air inlet (H), and corrosion-resistant filling is housed in the pipe, and tube hub is the center cooling tube.What link to each other with bromine charging aperture (I) is the bromine disperser, and effect is that bromine is evenly entered in the pipe.What link to each other with acetylene gas air inlet (H) is the acetylene gas distributor, and effect is that acetylene gas is evenly entered in the pipe.The effect of filler is to make bromine and acetylene gas full and uniform contact in pipe.The size of filler, loading density and highly determine according to raw material feed rate and product growing amount.
Described outer cooling tube is one to have the straight type cooling tube of coolant inlet (A), coolant outlet (J), and length equates that with tube length of reaction tube diameter is 1.5 times of reaction tube diameter.
Center cooling tube, reaction tube and outer cooling tube are by the resistant material manufacturing, and resistant material mainly is an inorganic material, comprise Pyrex, enamel, corrosion resisting alloy etc.
The corrosion-resistant filling of filling mainly is an inorganic material in the reaction tube, comprises Pyrex, enamel, corrosion resisting alloy etc.
Utilize above reactor, the present invention also provides a kind of synthetic method of tetrabromoethane, and described tetrabromoethane is got by carry out addition reaction in above-mentioned reactor by bromine and acetylene gas.In reactor, bromine enters reaction tube by the bromine charging aperture and moves from top to bottom under the gravity effect, acetylene gas enters reaction tube by the acetylene gas air inlet and moves from bottom to top by pressure, by the abundant counter current contacting of the filler effect generation tetrabromoethane that reacts, the bromine steam of volatilization continues on reaction tube top to react with acetylene gas in pipe for bromine and acetylene gas.The acetylene gas flow is 2-3 a times of bromine flow.The tetrabromoethane crude product that generates is shifted out by the reactor lower part discharging opening, is for further processing again.Unreacted micro-bromine and excessive acetylene gas are discharged by upper part discharge port, absorb unreacted bromine through absorber, and acetylene gas reclaims and uses.Feed cooling agent in center cooling tube and the outer cooling tube, and control the reaction tube interior reaction temperature by regulating coolant temperature and flow, cooling agent is mainly water, salt solution, methyl alcohol and ethanol etc.The ANALYSIS OF COOLANT FLOW direction is opposite with the acetylene gas flow direction.
The invention effect: of the present invention be used for bromine and acetylene gas carry out addition reaction prepare the reactor of tetrabromoethane and synthesis technique by bromine and acetylene gas continuous flow upstream haptoreaction in pipe, realized the synthetic continuously of tetrabromoethane, improved production efficiency, temperature by regulating cooling agent in the inside and outside cooling tube and flow are realized the control to reaction temperature, avoided that reaction temperature is too high causes danger and to the influence of addition reaction.
Description of drawings
Fig. 1 a kind ofly is used for bromine and acetylene gas carries out the reactor schematic diagram that addition reaction prepares tetrabromoethane.
The specific embodiment
The reacting appliance that used bromine and acetylene addition reaction prepare tetrabromoethane has following major parameter:
The reaction tube total length is 2.2m, and the filler loading height is 2m in the reaction tube, filling diameter in the tower
Pyrex Dixon ring type filler.Center cooling tube and outer cooling length of tube are respectively 2m.Center cooling tube diameter is 50mm, and reaction tube diameter is 100mm, and outer cooling tube diameter is 150mm.Reactor material is Pyrex.
The following describes the synthesis technique of tetrabromoethane, acetylene gas is by entering reaction tube and evenly in the distributor pipe by the acetylene gas distributor, and acetylene gas is bottom-up under pressure to be moved and be full of reaction tube, discharges air fully.Then, bromine enters reaction tube by charging aperture, and the bromine flow is 1Kg/h, make in the even distributor pipe of bromine by the bromine disperser, move down under the gravity effect, generate tetrabromoethane with acetylene gas counter current contacting generation addition reaction, the acetylene gas flow is 2 times of bromine flow.Feed 10 ℃ cooling water in center cooling tube and the outer cooling tube, flow direction is opposite with the acetylene gas flow direction, and the flow of regulating cooling water is to guarantee that reaction tube inner reaction tube temperature is less than 30 ℃.The tetrabromoethane crude product that flows out reaction tube obtains the tetrabromoethane product through neutralization and purification step.
Adopt above-mentioned reactor and synthesis technique, can realize the continuous addition reaction of bromine and acetylene gas, enhance productivity and productive rate, can avoid forming the explosive mixture of acetylene and air, improve reaction safety, simultaneously exothermic heat of reaction be can in time remove, too high safety problem of bringing of temperature and the too much problem of accessory substance solved.
Claims (4)
1. one kind is used for the reactor that bromine and acetylene addition reaction prepare tetrabromoethane, and critical piece is: the reaction tube (D) of center cooling tube (F), interior filling material, outer cooling tube (C), and appeal three critical pieces and be combined as reactor body.
Described center cooling tube is one to have the straight type cooling tube of coolant inlet (G), coolant outlet (K), and center cooling tube length equates that with tube length of reaction tube diameter is 1/3 of a reaction tube diameter.
Described reaction tube (D) is one to have the reaction tube of bromine charging aperture (I), acetylene gas air inlet (H), and the reaction tube center is the center cooling tube, and reaction tube is outward outer cooling tube.
Described outer cooling tube is one to have the straight type cooling tube of coolant inlet (A), coolant outlet (J), and length equates that with tube length of reaction tube diameter is 1.5 times of reaction tube diameter.
2. be used for the reactor that bromine and acetylene addition reaction prepare tetrabromoethane according to claim 1 a kind of, it is characterized in that: corrosion-resistant filling is housed in the reaction tube, and the material of filler is selected a kind of in the following material for use: Pyrex, enamel, corrosion resisting alloy.
3. be used for the reactor that bromine and acetylene addition reaction prepare tetrabromoethane according to claim 1 a kind of, it is characterized in that: the material of reactor is selected a kind of in the following material for use: Pyrex, enamel, corrosion resisting alloy.
4. synthetic method that is used for the tetrabromoethane of the described reactor of claim 1, it is characterized in that: bromine enters reaction tube by the bromine charging aperture, generate tetrabromoethane with the acetylene gas counter current contacting generation addition reaction that enters reaction tube by the acetylene gas air inlet, the acetylene gas flow is 2-3 a times of bromine flow, the tetrabromoethane crude product that generates is shifted out by the reactor lower part discharging opening, and unreacted micro-bromine and excessive acetylene gas are discharged by upper part discharge port; Feed cooling agent in center cooling tube and the outer cooling tube, control the reaction tube interior reaction temperature by regulating coolant flow.
Described cooling agent is selected for use following a kind of: water, salt solution, methyl alcohol and ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910256092A CN101766980A (en) | 2009-12-29 | 2009-12-29 | Reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and synthesis process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910256092A CN101766980A (en) | 2009-12-29 | 2009-12-29 | Reactor for preparing tetrabromoethane by addition reaction of bromine and acetylene and synthesis process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911941A (en) * | 2018-05-25 | 2018-11-30 | 凯莱英生命科学技术(天津)有限公司 | 1,3- cyclohexadiene is continuously synthesizing to method |
| CN110437027A (en) * | 2019-09-09 | 2019-11-12 | 马鞍山昂扬新材料科技有限公司 | A kind of production technology preparing tetrabromoethane using micro passage reaction |
| CN114315509A (en) * | 2021-12-28 | 2022-04-12 | 马鞍山昂扬新材料科技有限公司 | Safe low-waste tetrabromoethane production process |
-
2009
- 2009-12-29 CN CN200910256092A patent/CN101766980A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911941A (en) * | 2018-05-25 | 2018-11-30 | 凯莱英生命科学技术(天津)有限公司 | 1,3- cyclohexadiene is continuously synthesizing to method |
| CN110437027A (en) * | 2019-09-09 | 2019-11-12 | 马鞍山昂扬新材料科技有限公司 | A kind of production technology preparing tetrabromoethane using micro passage reaction |
| CN110437027B (en) * | 2019-09-09 | 2022-03-29 | 马鞍山昂扬新材料科技有限公司 | Production process for preparing tetrabromoethane by using microchannel reactor |
| CN114315509A (en) * | 2021-12-28 | 2022-04-12 | 马鞍山昂扬新材料科技有限公司 | Safe low-waste tetrabromoethane production process |
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