CN208532649U - Continuous production device for chloroacetic acid - Google Patents
Continuous production device for chloroacetic acid Download PDFInfo
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- CN208532649U CN208532649U CN201821008634.1U CN201821008634U CN208532649U CN 208532649 U CN208532649 U CN 208532649U CN 201821008634 U CN201821008634 U CN 201821008634U CN 208532649 U CN208532649 U CN 208532649U
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Abstract
The utility model discloses a kind of continuous production device for chloroacetic acid, there is the feed(raw material)inlet being located above and acyl chlorides refluxing opening, the chlorine disperser inside the gas vent of tower top, the chlorine inlet and tower body below tower body with chlorination tower, drainer, hydrogen chloride collection device, heating tank, semi-finished product tank, on the tower body of chlorination tower, positioned at the export of goods in process of manufacture of chlorination tower bottom.Monoxone side reaction product made from the utility model is few, and environmental pollution is few, high degree of automation, high production efficiency.
Description
Technical field
The utility model relates to chloroacetic production technologies.
Background technique
Traditional monoxone carries out reaction production using reaction kettle (or chlorination tank), and raw material is all added in reaction kettle and stops
Hair is stayed to answer the long period, reaction speed is difficult to control, and is easy excessively hair and is answered, generates the pairs such as more dichloroacetic acid, trichloroacetic acid
Product influences chloroacetic purity and the rate of output, and reaction kettle adding raw materials and the process of discharge product cannot be carried out continuously,
Cause production efficiency low.
In the chloroacetic article of continuous chlorination legal system of second phase nineteen ninety-five " chlorine industry " publication, describe with aceticanhydride
(acetic anhydride) is that catalyst carries out the chloroacetic technique of multistep reaction production, and reaction step is more, and by-product dichloroacetic acid is more, and product is pure
It spends lower.
A kind of production method of liquid chloroacetic acid of the disclosure of the invention of Patent No. 2012100386879, acetic acid is added
Chlorination tank, with chlorine reaction, generates monoxone in the presence of catalyst acetic anhydride, and reaction temperature is 70 DEG C, and the reaction time is 24 small
When.Application No. is a kind of large-scale chlorination tanks of 2012103848085 disclosure of the invention to produce chloroacetic technique, using three chlorine
Change kettle " two main one is secondary ", the tail gas after main still chlorination reaction is passed through secondary kettle and carries out chlorination reaction, the chlorination obtained after chlorination reaction
Liquid is crystallized, separates up to monoxone;After acetic acid and catalyst aceticanhydride are added in main still, collet is warming up to 85 DEG C, chlorine point
Three phases, which are passed through, is carried out continuously chlorination reaction.The two inventions be all made of closed reaction kettle and using aceticanhydride do catalyst into
Row reaction, reaction is discontinuous, and yield is relatively low, and by-products content is on the high side.
Summary of the invention
Purpose of utility model: it provides a kind of using dual catalyst catalysis, the monoxone that the reaction time is short, by-products content is few
Continuous production device.
Technical solution:
There is a kind of continuous production device for chloroacetic acid provided by the utility model chlorination tower, drainer, hydrogen chloride to collect
Device, heating tank, semi-finished product tank.On the tower body of chlorination tower have be located above feed(raw material)inlet, positioned at top gas vent,
Underlying chlorine inlet and therewith connection be located at chlorination tower in lower part chlorine disperser, positioned at chlorination tower bottom
Export of goods in process of manufacture (reaction product contains acetic acid when not yet purifying, becomes semi-finished product).
Feed(raw material)inlet (wherein containing acetic acid, aceticanhydride, aceticanhydride is as catalyst) connection feed conduit of chlorination tower, chlorine
(another raw material) has hydrogen chloride gas by chlorine inlet connection chlorine gas distributor, gas vent connection condenser, condenser
The chloroacetic chloride of body outlet and liquid exports;Export of goods in process of manufacture connection semi-finished product entrance.
Condenser uses graphite for main material, and corrosion resistance and heat conductivity are good, and controller condensation temperature (guarantees second
Acyl chlorides liquefaction, hydrogen chloride will not liquefy purer), chloroacetic chloride outlet is flowed back by the chloroacetic chloride of return line connection chlorination tower
Mouthful.
Acetic acid chloridising produces monoxone at present, and the overwhelming majority uses sulfur catalyst method, and a small number of producers use acetic anhydride catalysis
Method.There are no directly make catalyst using chloroacetic chloride.For chloroacetic chloride in the presence of strong acid, acylated ability is stronger than aceticanhydride, right
Chlorination reaction, which occurs, for carboxylic acid has catalytic action, that is, has better chlorination reaction catalysis.Acetyl in the utility model
Chlorine participates in chlorination reaction in the presence of having hydrogen chloride, by the catalyst that can be used as stronger catalytic capability, is then evaporated again from gas
Outlet discharge, uses as second of catalyst circulation, accelerates chlorination reaction velocity, when reducing the delay in raw material chlorination tower
Between, so that the phenomenon that chlorination reaction is less prone to overreact, reduces the generation of by-product;There is poison additionally, due to chloroacetic chloride
Property, pollution environment is easy in traditional handicraft when as byproduct emission, repeatedly reuse as catalyst while reduce and discharge.
Export of goods in process of manufacture, which distinguishes connection heating tank and monoxone semi-finished product tank, the outlet of heating tank by three-way valve, to be had
Return line connection semi-finished product entrance.There is Self-controlled pump between three-way valve and heating tank, connect between three-way valve and Self-controlled pump
It is connected to controller, Self-controlled pump has the component of chloroethene acid concentration in measurement semi-finished product.When chloroethene acid concentration is not less than in semi-finished product
When 80-85%, three-way valve is opened towards semi-finished product tank, collects semi-finished product;When chloroethene acid concentration is lower than 80-85%, threeway
Valve towards heating tank open, it is heated after reflux return chlorination tower so that not yet reaction so that raw material or intermediate product continue into
Row reaction.
The multiple sieve plate and the multiple filling layers below sieve plate that top in chlorination tower has layering setting;Feed(raw material)inlet
With multiple, chloroacetic chloride refluxing opening has multiple, and the sieve plate of connection different layers, multiple feed(raw material)inlets and multiple chloroacetic chlorides return respectively
Head piece position is arranged in a crossed manner.
Hydrogen chloride collection device includes vacuum jet package (devices) (discharge for accelerating hydrogen chloride), condenser, water replanishing device (quickening
The absorption of hydrogen chloride is dissolved), circulating pump, concentrated hydrochloric acid collection device, condenser has the top of return line connection injection apparatus
Entrance and lower part outlet, the upper entrance of water replanishing device connection injection apparatus, the lower part of concentrated hydrochloric acid collection device connection injection device
Outlet.
In the utility model, continuous rectification system can connect after semi-finished product tank, to obtain high-purity monoxone, realized
Continuous production of the raw material to high-purity monoxone finished product.
In the chlorination tower of the utility model, due to raw material and acetic anhydride catalysis agent using be continuously added to, semi-finished product, by-product etc.
In the chlorination tower for this vertical structure for flowing continually out, and using, when determining reaction due to gravity and the way of contact
Between short, liquid, gas quick separating, chlorine and acetic acid generally only occur step chemical reaction, there is intermediate production in single step reaction
Object chloroacetic chloride generates, it is difficult to instead give birth to deep reaction, by-product dichloro, trichlorine product seldom (structure of device makes reaction former
Material comes into full contact with, reaction sufficiently, even and if since the collective effect chlorination reaction time of two kinds of catalyst is shorter, chlorination reaction
Can smoothly complete, and will not react excessive and generate the harmful side products such as excessive dichloroacetic acid or trichloroacetic acid), it is chloroacetic pure
It spends higher.
The utility model has the advantages that
Traditional chlorinating container reaction, due to overreaction, by-product needs to pass through hydrogenating reduction.The utility model
Since the reaction time is short in equipment use, there is no the more phenomenons of overreact and by-product, do not need hydrogenation zone reduction two
The by products such as chlorine, trichlorine save the consumption of hydrogenation plant investment and feed hydrogen.
Continuous production is manually few, less energy consumption, and useful raw materials or intermediate include that catalyst is reused, and reduces equipment and throws
Enter the consumption with raw material.The reaction of dual catalytic agent catalytic chlorination, reaction speed is fast, and monoxone conversion ratio is higher.
Equipment heat transfer and corrosion resistance are strong, and service life is permanent.The concentration of reaction product can accurately control setting, produce
Impurity is less in object, and later purification is more convenient, and the very high monoxone of purity can be made.
Detailed description of the invention
A kind of process units of the utility model when Fig. 1.
In figure, 7- vacuum system;30- acetic acid and aceticanhydride raw material source;31- chlorine gas source;The feed(raw material)inlet 32-;33- chlorination tower;
34- sieve plate;35- filler;36- distributor;37- chloroacetic chloride refluxing opening;38- drainer;39- hydrochloric acid tank;40- heating tank;41- is certainly
Control pump;42- controller;43- triple valve;44- vapour source;45- condensed water collecting device;46- semi-finished product tank;47- semi-finished product go out
Mouthful;50- hydrogen chloride collection device
Specific embodiment
Continuous production device for chloroacetic acid as shown in Figure 1 has chlorination tower, drainer, hydrogen chloride collection device, heating
Tank, semi-finished product tank have the feed(raw material)inlet being located above, the gas vent positioned at top on the tower body of chlorination tower, separately have position
The chlorine disperser of chlorine inlet below chlorination tower and therewith connection being located inside chlorination tower, also has and is located at chlorination tower
The export of goods in process of manufacture of bottom.
Feed conduit passes through chlorine inlet connection chlorine gas distributor, gas by feed(raw material)inlet connection chlorination tower, chlorine pipeline
Body exports connection condenser, and condenser has hydrogen chloride gas outlet and the outlet of liquid chloroacetic chloride, and the condensation temperature of condenser is protected
Chloroacetic chloride liquefaction is demonstrate,proved, hydrogen chloride will not liquefy.Chloroacetic chloride outlet passes through the chloroacetic chloride refluxing opening of return line connection chlorination tower;Half
Product outlet connection semi-finished product tank.
Export of goods in process of manufacture distinguishes connection heating tank and semi-finished product tank by three-way valve, and the outlet of heating tank has return pipe
Road connection semi-finished product entrance;There is Self-controlled pump between three-way valve and heating tank, control is connected between three-way valve and Self-controlled pump
Device processed, Self-controlled pump have the function of that chloroethene acid concentration in semi-finished product can be measured.
The multiple sieve plate and the packing layer below sieve plate that top inside chlorination tower has layering setting;Feed(raw material)inlet
With multiple, chloroacetic chloride refluxing opening has multiple, and the sieve plate of connection different layers, multiple feed(raw material)inlets and multiple chloroacetic chlorides return respectively
Head piece position is arranged in a crossed manner.
Hydrogen chloride collection device includes vacuum jet package (devices), condenser, water replanishing device, circulating pump, concentrated hydrochloric acid collection device,
Condenser has the upper entrance and lower part outlet of return line connection injection apparatus, the top of water replanishing device connection injection apparatus
Entrance, the lower part outlet of concentrated hydrochloric acid collection device connection injection device.
Claims (6)
1. a kind of continuous production device for chloroacetic acid has chlorination tower, drainer, hydrogen chloride collection device, heating tank, semi-finished product
Tank has the feed(raw material)inlet being located above, the gas vent positioned at top on the tower body of chlorination tower, it is characterised in that: separately have
The chlorine disperser of chlorine inlet below chlorination tower and therewith connection being located inside chlorination tower, also has and is located at chlorination
The export of goods in process of manufacture of tower bottom;
Feed conduit is gone out by feed(raw material)inlet connection chlorination tower, chlorine pipeline by chlorine inlet connection chlorine gas distributor, gas
Mouth connection condenser, condenser have hydrogen chloride gas outlet and the outlet of liquid chloroacetic chloride, and chloroacetic chloride, which exports, passes through return line
The chloroacetic chloride refluxing opening of connection chlorination tower;Export of goods in process of manufacture connection semi-finished product tank.
2. continuous production device for chloroacetic acid as described in claim 1, it is characterised in that: condenser uses graphite for main material
Matter.
3. continuous production device for chloroacetic acid as described in claim 1, it is characterised in that: export of goods in process of manufacture passes through three-way valve
The outlet of connection heating tank and semi-finished product tank respectively, heating tank has return line connection semi-finished product entrance;Three-way valve with plus
There is Self-controlled pump between hot tank, be connected with controller between three-way valve and Self-controlled pump, Self-controlled pump has and can measure semi-finished product
The function of middle chloroethene acid concentration.
4. continuous production device for chloroacetic acid as claimed in claim 1,2 or 3, it is characterised in that: the top inside chlorination tower
Multiple sieve plate with layering setting and the packing layer below sieve plate;Feed(raw material)inlet has multiple, chloroacetic chloride refluxing opening tool
Have it is multiple, respectively connection different layers sieve plate, multiple feed(raw material)inlets and multiple chloroacetic chloride refluxing openings position are arranged in a crossed manner.
5. continuous production device for chloroacetic acid as described in claim 1, it is characterised in that: hydrogen chloride collection device includes vacuum
Injection apparatus, condenser, water replanishing device, circulating pump, concentrated hydrochloric acid collection device, condenser have return line connection injection apparatus
Upper entrance and lower part outlet, the upper entrance of water replanishing device connection injection apparatus, concentrated hydrochloric acid collection device connection injection device
Lower part outlet.
6. continuous production device for chloroacetic acid as described in claim 1, it is characterised in that: be connected with after semi-finished product tank continuous
Distillation system.
Priority Applications (1)
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CN201821008634.1U CN208532649U (en) | 2018-06-28 | 2018-06-28 | Continuous production device for chloroacetic acid |
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CN201821008634.1U CN208532649U (en) | 2018-06-28 | 2018-06-28 | Continuous production device for chloroacetic acid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108484386A (en) * | 2018-06-28 | 2018-09-04 | 南通山剑石墨设备有限公司 | Continuous production device for chloroacetic acid and its production technology |
CN110975475A (en) * | 2019-12-06 | 2020-04-10 | 莘县华祥盐化有限公司 | Chloroacetic acid sheeting packaging dust recycling system and method |
-
2018
- 2018-06-28 CN CN201821008634.1U patent/CN208532649U/en active Active
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108484386A (en) * | 2018-06-28 | 2018-09-04 | 南通山剑石墨设备有限公司 | Continuous production device for chloroacetic acid and its production technology |
CN110975475A (en) * | 2019-12-06 | 2020-04-10 | 莘县华祥盐化有限公司 | Chloroacetic acid sheeting packaging dust recycling system and method |
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Effective date of registration: 20230410 Address after: 226000 No.80 Yuwan Middle Road, Shigang Town, Tongzhou District, Nantong City, Jiangsu Province Patentee after: NANTONG SHANJIAN ANTICORROSIVE TECHNOLOGY CO.,LTD. Address before: 226003 No. 815, city road, Nantong, Jiangsu Patentee before: NANTONG SHAN JIAN GRAPHITE EQUIPMENT Co.,Ltd. |