CN108299306A - A kind of tail gas treatment process in bromochloroin building-up process - Google Patents
A kind of tail gas treatment process in bromochloroin building-up process Download PDFInfo
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- CN108299306A CN108299306A CN201810297278.8A CN201810297278A CN108299306A CN 108299306 A CN108299306 A CN 108299306A CN 201810297278 A CN201810297278 A CN 201810297278A CN 108299306 A CN108299306 A CN 108299306A
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- tail gas
- gas absorption
- bromochloroin
- kettle
- liquid
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Links
- 238000000034 method Methods 0.000 title claims abstract description 38
- 230000008569 process Effects 0.000 title claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 204
- 238000010521 absorption reaction Methods 0.000 claims abstract description 184
- 239000007788 liquid Substances 0.000 claims abstract description 132
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 79
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 75
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 74
- 238000010828 elution Methods 0.000 claims abstract description 55
- 239000012452 mother liquor Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 50
- 239000000460 chlorine Substances 0.000 claims description 50
- 229910052801 chlorine Inorganic materials 0.000 claims description 50
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 35
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 35
- 229910052794 bromium Inorganic materials 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- 229910001868 water Inorganic materials 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 29
- 150000001875 compounds Chemical class 0.000 claims description 23
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 230000007613 environmental effect Effects 0.000 claims description 11
- 238000010189 synthetic method Methods 0.000 claims description 11
- 238000005893 bromination reaction Methods 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 230000031709 bromination Effects 0.000 claims description 7
- 238000005660 chlorination reaction Methods 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000002140 halogenating effect Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- -1 Dimethyl Hydan Chemical compound 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 127
- 238000003756 stirring Methods 0.000 description 24
- 238000001035 drying Methods 0.000 description 6
- 210000003298 dental enamel Anatomy 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000012795 verification Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- ORIYNSKCWVSBFJ-UHFFFAOYSA-N C(CO)(=O)NC(=O)N.[Br] Chemical compound C(CO)(=O)NC(=O)N.[Br] ORIYNSKCWVSBFJ-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- ZHLKXBJTJHRTTE-UHFFFAOYSA-N Chlorobenside Chemical compound C1=CC(Cl)=CC=C1CSC1=CC=C(Cl)C=C1 ZHLKXBJTJHRTTE-UHFFFAOYSA-N 0.000 description 1
- 241000195493 Cryptophyta Species 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 125000000950 dibromo group Chemical group Br* 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical class O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009182 swimming Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/54—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members
- C07D233/66—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D233/72—Two oxygen atoms, e.g. hydantoin
- C07D233/80—Two oxygen atoms, e.g. hydantoin with hetero atoms or acyl radicals directly attached to ring nitrogen atoms
- C07D233/82—Halogen atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
The present invention relates to the tail gas treatment process in a kind of bromochloroin building-up process comprising following steps, 1. prepare bromochloroin for raw material with 5,5 Dimethyl Hydan in synthesis reactor；Synthesis reactor tail gas is passed through tail gas absorption kettle, and tail gas absorption kettle is emptied through environmentally friendly absorption tower；It is provided with tail gas absorption liquid in tail gas absorption kettle, is the aqueous solution or 5 of 5,5 Dimethyl Hydan and sodium hydroxide, the mixed liquor of the C5H6Br2N2O2 mother liquor of 5 Dimethyl Hydan and sodium hydroxide；It is provided with elution absorbing liquid in environmentally friendly absorption tower, is the mixture of sodium hydrate aqueous solution or sodium hydroxide and C5H6Br2N2O2 mother liquor；2. after synthesis reactor sky kettle, the tail gas absorption liquid in tail gas absorption kettle is transferred in synthesis reactor, and interior elution absorbing liquid is transferred in tail gas absorption kettle and 5,5 Dimethyl Hydan are added in environmentally friendly absorption tower.The present invention makes the tail gas that bromochloroin building-up process generates, and is absorbed through tail gas absorption kettle, environmentally friendly absorption tower two-stage, has reached environment protection emission requirement.
Description
Technical field
The invention belongs to organic synthesis fields, and in particular to the tail gas treatment process in a kind of bromochloroin building-up process.
Background technology
Bromochloroin, chloro- 5, the 5- Dimethyl Hydan of the bromo- 3- of full name 1-；Chloro- 5, the 5- dimethyl hydantoins of the bromo- 3- of 1- are
White or off-white color crystalline powder, slightly chlorine flavor are dissolved in benzene, dichloromethane and chloroform, can be further processed into particle and
Tablet.Bromochloroin is oxidized form disinfectant of new generation, collects bromine chlorbenside bacterium advantage, compared with other chlorinated products, is had steady
Qualitative height, smell is small, fungicidal effectiveness is stronger and it is long to have the characteristics that slow release, validity continue, and can be widely used for：Swimming pool
And the sterilizing of drinking water；Culture fishery water body disinfection；Industrial circulating cooling water sterilization algae removal；Hotel, hospital etc. are public
Site surrounding sterilizes.Chinese Enterprises produce bromochloroin at present, mainly with 5,5- Dimethyl Hydan, sodium hydroxide, bromine or two
Bromine glycolylurea mother liquor（Aqueous sodium bromide）, chlorine be raw material, by the method for publicity, such as CN103333115A；CN101103723A；
CN1611492A etc.,
Its chemical equation is：
In enamel reaction still bromochloroin is synthesized under certain temperature.A kind of any of the above described bromochloroin synthetic method, contains chlorine
The synthesis tail gas processing method of gas is that synthesis tail gas is passed directly into environmental protection type sprinkling tower, is emptied after absorbing chlorine with lye, is produced
Raw a large amount of tail gas absorption waste liquid, is unfavorable for environmental protection, while also increasing production cost.
Invention content
The object of the present invention is to provide the tail gas treatment process in a kind of bromochloroin building-up process, use this technique place
After reason, there is no the generations of tail gas absorption waste liquid, are conducive to environmental protection, while the chlorine in tail gas is utilized again,
Chlorine utilization is improved, cost is reduced.
To achieve the above object, the present invention provides the tail gas treatment process in a kind of bromochloroin building-up process, packets
Include following steps comprising following steps,
（1）Bromochloroin is prepared in synthesis reactor using 5,5- Dimethyl Hydan as raw material；The tail gas of the synthesis reactor is passed through tail gas
In absorption kettle, the evacuated tube of the tail gas absorption kettle is emptied through environmentally friendly absorption tower；Tail gas suction is provided in the tail gas absorption kettle
Liquid is received, the tail gas absorption liquid is the aqueous solution or 5 of 5,5- Dimethyl Hydan and sodium hydroxide, 5- Dimethyl Hydan and hydroxide
The mixed liquor of the C5H6Br2N2O2 mother liquor of sodium；
Elution absorbing liquid is provided in the environmental protection absorption tower, the elution absorbing liquid is sodium hydrate aqueous solution or sodium hydroxide
With the mixture of C5H6Br2N2O2 mother liquor；
（2）Work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle turns
Enter in synthesis reactor, synthesizes bromochloroin, while elution absorbing liquid interior in environmentally friendly absorption tower is transferred in tail gas absorption kettle and is added
Step（1）5, the 5- Dimethyl Hydan of synthetic ratio, the tail gas absorption liquid as tail gas absorption kettle use；In environmentally friendly absorption tower
Elution absorbing liquid is prepared again.
Further, step（1）It is middle prepare bromochloroin synthetic method be,
It routinely matches 5,5- Dimethyl Hydan and sodium hydroxide is soluble in water, uses bromine and chlorine as halogenating agent, carry out
Bromination and chlorination reaction；
The tail gas absorption liquid is to add 5,5- Dimethyl Hydan, sodium hydroxide and water by synthetic ratio；
The elution absorbing liquid is to add sodium hydroxide and water by synthetic ratio.
Further, step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, tail gas is inhaled
The tail gas absorption liquid received in kettle is transferred in synthesis reactor, according to step in synthesis reactor（1）In proportioning, be added dropwise and bromine and be passed through chlorine
Gas synthesizes bromochloroin again；Elution absorbing liquid in environmentally friendly absorption tower is transferred in tail gas absorption kettle, and according to step（1）In
5,5- Dimethyl Hydan is added in proportioning, and the tail gas absorption liquid as tail gas absorption kettle uses；Elution in environmentally friendly absorption tower absorbs
Liquid is prepared again.
Further, step（1）The middle synthetic method for preparing bromochloroin is routinely to match 5,5- dimethyl sea
The sodium hydroxide of the 15-25% of cause and processing compound amount total weight is soluble in water, and bromine is added dropwise into this solution and is passed through chlorine
Meanwhile remaining sodium hydrate aqueous solution is added dropwise；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, the 15- of water and processing compound amount total weight
25% sodium hydroxide mixture；
The elution absorbing liquid is that the sodium hydroxide of the 15-25% of the water and processing compound amount total weight that are prepared by synthetic ratio is mixed
Close object；
Further, step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, tail gas absorption kettle
Interior tail gas absorption liquid is transferred in synthesis reactor, according to step in synthesis reactor（1）In proportioning be added dropwise and bromine and be passed through chlorine
Meanwhile a dropping step（1）The sodium hydroxide of the middle remaining 75%-85% of processing compound amount total weight, synthesizes bromochloroin again；Together
Elution absorbing liquid in the absorption towers Shi Huanbao is transferred in tail gas absorption kettle and step is added（1）The 5,5- dimethyl of synthetic ratio
Glycolylurea, the tail gas absorption liquid as tail gas absorption kettle use；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
Further, step（1）The middle synthetic method for preparing bromochloroin is routinely to match 5,5- dimethyl sea
It is dissolved in the mother liquor containing sodium bromide that cause is generated when producing C5H6Br2N2O2, uses chlorine as halogenating agent, while quality is added dropwise
Score is that 30-37% sodium hydroxide solutions carry out bromination and chlorination reaction；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, mother liquor and processing compound containing sodium bromide
The mass fraction for measuring the 15-25% of total weight is the sodium hydroxide solution mixture of 30-37%；
The elution absorbing liquid is that the mass fraction of the water prepared by synthetic ratio and processing compound amount total weight 15-25% are 30-
37% sodium hydroxide solution mixture.
Further, the mother liquor containing sodium bromide that generates is when producing C5H6Br2N2O2：With 5,5- Dimethyl Hydan, hydrogen-oxygen
Change sodium, bromine is raw material, molar ratio 1：（2.0-2.1）：（2.0-2.2）, in aqueous solution, controlling reaction temperature is at -5 DEG C
To 35 DEG C, bromine is added dropwise and carries out bromination reaction, after the completion of reaction, it is dibromo that C5H6Br2N2O2, remaining liquid are removed in centrifugation
Glycolylurea mother liquor.
Further, step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, tail gas is inhaled
The tail gas absorption liquid received in kettle is transferred in synthesis reactor, and chlorine, while a dropping step are passed through in synthesis reactor（1）Middle processing compound amount
The mass fraction of the remaining 75%-85% of total weight is 30-37% sodium hydroxide solutions, synthesizes bromochloroin again；Environmental protection is inhaled simultaneously
The elution absorbing liquid received in tower is transferred in tail gas absorption kettle and step is added（1）5, the 5- Dimethyl Hydan of synthetic ratio is made
It is used for the tail gas absorption liquid of tail gas absorption kettle；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
Further, the tail gas absorption liquid pH value in the tail gas absorption kettle is 12 or more；Control material in tail gas absorption kettle
Liquid temperature is at 5-15 DEG C.
Further, the elution absorbing liquid pH value in the environmentally friendly absorption tower is 12 or more.
Further, the tail gas absorption liquid pH value in the tail gas absorption kettle is 12-14；
Further, the elution absorption liquid pH in the environmentally friendly absorption tower is 13-14.
Good effect of the present invention is as follows：
（1）The tail gas that bromochloroin building-up process generates absorbs through tail gas absorption kettle, environmentally friendly absorption tower two-stage, has reached environmental protection
Emission request.
（2）The elution absorbing liquid in tail gas absorption liquid and environmentally friendly absorption tower in tail gas absorption kettle is used as synthesis material,
It is fully used.There is no the generations of tail gas absorption waste liquid, are conducive to environmental protection.The chlorine in tail gas obtains again simultaneously
Utilization has been arrived, chlorine utilization is improved, has reduced cost.
Specific implementation mode
It will make further narration in detail to the embodiment of the present invention below.
The present invention is with reference to patent CN103333115A；CN101103723A；The bromochloroin synthetic method such as CN1611492A
Proportioning and technical process.
The present invention includes the following steps comprising following steps,
（1）Bromochloroin is prepared in synthesis reactor using 5,5- Dimethyl Hydan as raw material；The tail gas of the synthesis reactor is passed through tail gas
In absorption kettle, the evacuated tube of the tail gas absorption kettle is emptied through environmentally friendly absorption tower；Tail gas suction is provided in the tail gas absorption kettle
Liquid is received, the tail gas absorption liquid is the aqueous solution or 5 of 5,5- Dimethyl Hydan and sodium hydroxide, 5- Dimethyl Hydan and hydroxide
The mixed liquor of the C5H6Br2N2O2 mother liquor of sodium；
Elution absorbing liquid is provided in the environmental protection absorption tower, the elution absorbing liquid is sodium hydrate aqueous solution or sodium hydroxide
With the mixture of C5H6Br2N2O2 mother liquor；
（2）Work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle turns
Enter in synthesis reactor, synthesizes bromochloroin, while elution absorbing liquid interior in environmentally friendly absorption tower is transferred in tail gas absorption kettle and is added
Step（1）5, the 5- Dimethyl Hydan of synthetic ratio, the tail gas absorption liquid as tail gas absorption kettle use；In environmentally friendly absorption tower
Elution absorbing liquid is prepared again.
Embodiment 1
The synthesis of this example bromochloroin conventionally carries out.With 5,5- Dimethyl Hydan, water, sodium hydroxide, bromine and
Chlorine is raw material.First according to preset ratio, keeps 5,5- Dimethyl Hydan and whole sodium hydroxides soluble in water, control a constant temperature
Bromine is added dropwise in degree, is passed through chlorine, carries out bromination and chlorination reaction.Halogenated products are centrifuged, wash, and are dried and are made
Bromochloroin.
Step（1）It is middle prepare bromochloroin synthetic method be,
It routinely matches 5,5- Dimethyl Hydan and sodium hydroxide is soluble in water, uses bromine and chlorine as halogenating agent, carry out
Bromination and chlorination reaction；
The tail gas absorption liquid is to add 5,5- Dimethyl Hydan, sodium hydroxide and water by synthetic ratio；
The elution absorbing liquid is to add sodium hydroxide and water by synthetic ratio.
Step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail in tail gas absorption kettle
Aspiration liquid is transferred in synthesis reactor, according to step in synthesis reactor（1）In proportioning, bromine is added dropwise and is passed through chlorine and synthesizes again
Bromochloroin；Elution absorbing liquid in environmentally friendly absorption tower is transferred in tail gas absorption kettle, and according to step（1）Middle proportioning is added 5,
5- Dimethyl Hydan, the tail gas absorption liquid as tail gas absorption kettle use；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
Specifically：
A, 1600kg water is added in 2000L enamel synthesis reaction vessels, starts stirring, control material temperature in kettle adds at 5-9 DEG C
Enter 120kg 5,5- Dimethyl Hydan, 75kg flaky sodium hydrates, stirring and dissolving.Brine ice cooling simultaneously.When object in synthesis reactor
Material temperature degree is down to 5 DEG C, and bromine 75kg is added dropwise.After the completion of bromine dropwise adding, stir 15 minutes.Then control material temperature in kettle is in 5-
10 DEG C, it is passed through chlorine 100kg.It after chlorine has led to, stirs 30 minutes, material centrifugal dewatering is washed with water 115kg, dehydration, 50-
80 DEG C of dryings, obtain bromochloroin 218kg.Yield 96.3%, content 99.5%.
The tail gas of above-mentioned reaction is passed through in 2000L tail gas absorption kettles.Tail gas absorption kettle inner exhaust gas absorbing liquid is：1600kg water
Middle addition 120kg 5,5- Dimethyl Hydan, 75kg sodium hydroxides, stirring and dissolving.Temperature is controlled at 5-15 DEG C.Tail gas absorption liquid
PH value is 14.
The evacuated tube of tail gas absorption kettle passes to environmentally friendly absorption tower.The elution absorbing liquid on environmentally friendly absorption tower is：In 1600kg water
75kg sodium hydroxides, stirring and dissolving is added.Tail gas absorption liquid pH value is 14.
B, synthesis reactor completes discharging in a, and after empty kettle, tail gas absorption kettle inner exhaust gas absorbing liquid is turned material to synthesis reactor,
According to step in synthesis reactor（1）In proportioning, bromine is added dropwise and is passed through chlorine and synthesizes bromochloroin again.Elution is inhaled in environmentally friendly tower
It receives liquid and goes to tail gas absorption kettle, 120kg 5,5- Dimethyl Hydan, stirring and dissolving is added.Temperature is controlled at 5-15 DEG C.Environmentally friendly tower
Interior elution absorbing liquid is prepared again with a.
In order to illustrate the bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality is unaffected.
The present embodiment has further done following verification：
When synthesis material temperature in kettle is down to 5 DEG C, bromine 75kg is added dropwise.After the completion of bromine dropwise adding, stir 15 minutes.Then it controls
Material temperature in kettle processed is passed through chlorine 94kg at 5-10 DEG C（Tail gas absorption liquid and environmentally friendly absorbing liquid have absorbed chlorine 6kg）, chlorine
It after gas has led to, stirs 30 minutes, material centrifugal dewatering is washed with water 115kg, and dehydration, 50-80 DEG C of drying obtains bromochloroin
217.5kg.Yield 96.1%, content 99.6%.
C, after the completion of b, b operations is repeated, bromochloroin 218.5kg, yield 96.5%, content 99.4% are obtained.Explanation
The bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality are unaffected.
Embodiment 2：
The synthesis of the present embodiment bromochloroin conventionally carries out.With 5,5- Dimethyl Hydan, water, sodium hydroxide, bromine
It is raw material with chlorine.Step（1）The middle synthetic method for preparing bromochloroin be routinely match 5,5- Dimethyl Hydan and
The sodium hydroxide of the 15-25% of processing compound amount total weight is soluble in water, and bromine is added dropwise into this solution and is passed through the same of chlorine
When, remaining sodium hydrate aqueous solution is added dropwise；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, the 15- of water and processing compound amount total weight
25% sodium hydroxide mixture；
The elution absorbing liquid is that the sodium hydroxide of the 15-25% of the water and processing compound amount total weight that are prepared by synthetic ratio is mixed
Close object.
Step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail in tail gas absorption kettle
Aspiration liquid is transferred in synthesis reactor, according to step in synthesis reactor（1）In proportioning bromine is added dropwise and while be passed through chlorine, drop
Add step（1）The sodium hydroxide of the middle remaining 75%-85% of processing compound amount total weight, synthesizes bromochloroin again；Environmental protection simultaneously
Elution absorbing liquid in absorption tower is transferred in tail gas absorption kettle and step is added（1）5, the 5- Dimethyl Hydan of synthetic ratio,
Tail gas absorption liquid as tail gas absorption kettle uses；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
Specifically：
D, 5,5- Dimethyl Hydan 135kg, 32% (weight percent) sodium hydroxide are added in 2000L enamel reaction stills
50kg, water 1000kg, stirring and dissolving.Material temperature in kettle is controlled at 5-9 DEG C, bromine 84kg is added dropwise.It is stirred after the completion of bromine dropwise adding
It mixes 30 minutes.5-9 DEG C of temperature control is passed through chlorine 113kg.Bromine is added dropwise and is passed through chlorine while being added dropwise 32%（Weight percent）Hydrogen
Sodium hydroxide solution amounts to 214kg.It after sodium hydroxide solution is added dropwise to complete, stirs 10 minutes, continues to be passed through chlorine 5kg, stirring is anti-
It answers 30 minutes.Reaction mass is through centrifugal dewatering, 110kg washings, 60-80 DEG C of drying, obtains bromochloroin 245kg, yield 96.2%,
Content 99.5%.
Above-mentioned synthesis reaction vessel offgas duct is passed through in 2000L tail gas absorption kettles.Tail gas absorption kettle inner exhaust gas absorbing liquid is：
Addition 135kg 5 in 1000kg water, 5- Dimethyl Hydan, 32%（Weight percent）Sodium hydroxide solution 50kg, stirring and dissolving.
Temperature is controlled at 5-15 DEG C.Tail gas absorption liquid pH value is 14.
The evacuated tube of tail gas absorption kettle passes to environmentally friendly absorption tower.The elution absorbing liquid on environmentally friendly absorption tower is：In 1000kg water
It is added 32%（Weight percent）Sodium hydroxide solution 50kg, stirring and dissolving.Tail gas absorption liquid pH value is 14.
E, synthesis reactor completes discharging in d, and after empty kettle, tail gas absorption kettle inner exhaust gas absorbing liquid is turned material to synthesis reactor,
According to step in synthesis reactor（1）In proportioning bromine is added dropwise and while be passed through chlorine, a dropping step（1）Middle processing compound amount is total
The sodium hydroxide 214kg of the 75%-85% of weight left synthesizes bromochloroin again.Elution absorbing liquid goes to tail gas suction in environmentally friendly tower
Kettle is received, 5, the 5- Dimethyl Hydan of 135kg, stirring and dissolving is added, the tail gas absorption liquid as tail gas absorption kettle uses.Control temperature
Degree is at 5-15 DEG C.Elution absorbing liquid is prepared again with d in environmentally friendly tower.
In order to illustrate the bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality is unaffected.
The present embodiment has further done following verification：
When synthesis material temperature in kettle is at 5-9 DEG C, while 32% being added dropwise in proportion（Weight percent）Sodium hydroxide solution 124kg,
Bromine 84kg,（Because including sodium hydroxide in tail gas absorption liquid and environmentally friendly leacheate and having absorbed 6kg chlorine, therefore bromine is added dropwise
The sodium hydroxide solution amount being added dropwise when plain and logical chlorine is reduced, and chlorine has also led to 6kg less）, bromine dropwise adding 30 points of stirring after the completion
Clock.5-9 DEG C of temperature control, while being added dropwise 32%（Weight percent）Sodium hydroxide solution 124kg is passed through chlorine 107kg.Sodium hydroxide
After solution is added dropwise to complete, stirs 10 minutes, continue to be passed through chlorine 5kg, be stirred to react 30 minutes.Reaction mass through centrifugal dewatering,
110kg is washed, and 60-80 DEG C of drying obtains bromochloroin 244.6kg, yield 96.0%, content 99.6%.
F, after the completion of e, e operations is repeated, bromochloroin 245.2kg, yield 96.3%, content 99.2% are obtained.Explanation
The bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality are unaffected.
Embodiment 3：
The synthesis of the present embodiment bromochloroin conventionally carries out.Step（1）It is middle prepare bromochloroin synthetic method be,
Routinely matching will dissolve in the mother liquor containing sodium bromide that 5,5- Dimethyl Hydan is generated when producing C5H6Br2N2O2, use chlorine
As halogenating agent, while it is that 30-37% sodium hydroxide solutions carry out bromination and chlorination reaction that mass fraction, which is added dropwise,；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, mother liquor and processing compound containing sodium bromide
The mass fraction for measuring the 15-25% of total weight is the sodium hydroxide solution mixture of 30-37%；
The elution absorbing liquid is that the mass fraction of the water prepared by synthetic ratio and processing compound amount total weight 15-25% are 30-
37% sodium hydroxide solution mixture.
Producing the mother liquor containing sodium bromide generated when C5H6Br2N2O2 is：With 5,5- Dimethyl Hydan, sodium hydroxide, bromine
For raw material, molar ratio 1：（2.0-2.1）：（2.0-2.2）, in aqueous solution, controlling reaction temperature is at -5 DEG C to 35 DEG C, drop
Bromine is added to carry out bromination reaction, after the completion of reaction, it is C5H6Br2N2O2 mother liquor that C5H6Br2N2O2, remaining liquid are removed in centrifugation.
Step（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail in tail gas absorption kettle
Aspiration liquid is transferred in synthesis reactor, and chlorine, while a dropping step are passed through in synthesis reactor（1）Middle processing compound amount total weight is remaining
75%-85% mass fraction be 30-37% sodium hydroxide solutions, synthesize bromochloroin again；Simultaneously in environmentally friendly absorption tower in
Elution absorbing liquid is transferred in tail gas absorption kettle and step is added（1）5, the 5- Dimethyl Hydan of synthetic ratio, as tail gas absorption
The tail gas absorption liquid of kettle uses；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
Specifically：
G, it is added 5,5- Dimethyl Hydan 135kg in 2000L enamel reaction stills, 11%（Weight percent）C5H6Br2N2O2 mother liquor
980kg, stirring and dissolving.Material temperature in kettle is controlled at 5-9 DEG C, while 32% being added dropwise in proportion（Weight percent）Sodium hydroxide
Solution 264kg is passed through chlorine 152kg.After sodium hydroxide solution is added dropwise to complete, stirs 10 minutes, continue to be passed through chlorine 5kg, stir
Mix reaction 30 minutes.Reaction mass obtains bromochloroin 245kg, yield through centrifugal dewatering, 110kg washings, 60-80 DEG C of drying
96.2%, content 99.5%.
Above-mentioned synthesis reaction vessel offgas duct is passed through in 2000L tail gas absorption kettles.Tail gas absorption kettle inner exhaust gas absorbing liquid is：
980kg 11%（Weight percent）C5H6Br2N2O2 mother liquor addition 135kg 5,5- Dimethyl Hydan, 32%（Weight percent）Hydrogen-oxygen
Change sodium solution 50kg, stirring and dissolving.Temperature is controlled at 5-15 DEG C.Tail gas absorption liquid pH value is 14.
The evacuated tube of tail gas absorption kettle passes to environmentally friendly absorption tower.The elution absorbing liquid on environmentally friendly absorption tower is：980kg 11%
（Weight percent）C5H6Br2N2O2 mother liquor is added 32%（Weight percent）Sodium hydroxide solution 50kg, stirring and dissolving.Tail gas absorption
Liquid pH value is 14.
H, synthesis reactor completes discharging in g, and after empty kettle, tail gas absorption kettle inner exhaust gas absorbing liquid is turned material to synthesis reactor,
Chlorine, while a dropping step are passed through in synthesis reactor（1）The middle remaining mass fraction of processing compound amount total weight is 30-37% hydrogen-oxygens
Change sodium solution 214g, synthesizes bromochloroin again.Elution absorbing liquid goes to tail gas absorption kettle in environmentally friendly tower, and 135kg5,5- is added
Dimethyl Hydan, stirring and dissolving.Temperature is controlled at 5-15 DEG C.Elution absorbing liquid is prepared again with g in environmentally friendly tower.
In order to illustrate the bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality is unaffected.
The present embodiment has further done following verification：
Synthesis material temperature in kettle is down to 5-9 DEG C, while 32% being added dropwise in proportion（Weight percent）Sodium hydroxide solution 214kg,
It is passed through chlorine 141kg.After sodium hydroxide solution is added dropwise to complete, stirs 10 minutes, continue to be passed through chlorine 5kg, be stirred to react 30 points
Clock.Reaction mass obtains bromochloroin 245.2kg, yield 96.3%, content through centrifugal dewatering, 110kg washings, 60-80 DEG C of drying
99.2%。
J, after the completion of h, h operations is repeated, bromochloroin 244.8kg, yield 96.1%, content 99.6% are obtained.Explanation
The bromochloroin synthesized with tail gas absorption liquid in tail gas absorption kettle, bromochloroin quality are unaffected.
The present invention（1）The tail gas that bromochloroin building-up process generates is absorbed through tail gas absorption kettle, environmentally friendly absorption tower two-stage,
Environment protection emission requirement is reached.
（2）The elution absorbing liquid in tail gas absorption liquid and environmentally friendly absorption tower in tail gas absorption kettle is used as synthesis material,
It is fully used.There is no the generations of tail gas absorption waste liquid, are conducive to environmental protection.The chlorine in tail gas obtains again simultaneously
Utilization has been arrived, chlorine utilization is improved, has reduced cost.
The foregoing is merely the section Examples of the present invention, are not intended to limit the invention.All essences in the present invention
All any modification, equivalent and improvement made by within refreshing and principle, should all be included in the protection scope of the present invention.
Claims (10)
1. the tail gas treatment process in a kind of bromochloroin building-up process, it is characterised in that：It includes the following steps,
（1）Bromochloroin is prepared in synthesis reactor using 5,5- Dimethyl Hydan as raw material；The tail gas of the synthesis reactor is passed through tail gas
In absorption kettle, the evacuated tube of the tail gas absorption kettle is emptied through environmentally friendly absorption tower；Tail gas suction is provided in the tail gas absorption kettle
Liquid is received, the tail gas absorption liquid is the aqueous solution or 5 of 5,5- Dimethyl Hydan and sodium hydroxide, 5- Dimethyl Hydan and hydroxide
The mixed liquor of the C5H6Br2N2O2 mother liquor of sodium；
Elution absorbing liquid is provided in the environmental protection absorption tower, the elution absorbing liquid is sodium hydrate aqueous solution or sodium hydroxide
With the mixture of C5H6Br2N2O2 mother liquor；
（2）Work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle turns
Enter in synthesis reactor, synthesizes bromochloroin, while elution absorbing liquid interior in environmentally friendly absorption tower is transferred in tail gas absorption kettle and is added
Step（1）5, the 5- Dimethyl Hydan of synthetic ratio, the tail gas absorption liquid as tail gas absorption kettle use；In environmentally friendly absorption tower
Elution absorbing liquid is prepared again.
2. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 1, it is characterised in that：Step
（1）It is middle prepare bromochloroin synthetic method be,
It routinely matches 5,5- Dimethyl Hydan and sodium hydroxide is soluble in water, uses bromine and chlorine as halogenating agent, carry out
Bromination and chlorination reaction；
The tail gas absorption liquid is to add 5,5- Dimethyl Hydan, sodium hydroxide and water by synthetic ratio；
The elution absorbing liquid is to add sodium hydroxide and water by synthetic ratio.
3. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 2, it is characterised in that：Step
（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle is transferred to
In synthesis reactor, according to step in synthesis reactor（1）In proportioning, bromine is added dropwise and is passed through chlorine and synthesizes bromochloroin again；Ring
The elution absorbing liquid protected in absorption tower is transferred in tail gas absorption kettle, and according to step（1）5,5- dimethyl sea is added in middle proportioning
Cause, the tail gas absorption liquid as tail gas absorption kettle use；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
4. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 1, it is characterised in that：Step
（1）The middle synthetic method for preparing bromochloroin is routinely to match 5,5- Dimethyl Hydan and processing compound amount total weight
The sodium hydroxide of 15-25% is soluble in water, and while bromine is added dropwise into this solution and is passed through chlorine, remaining hydroxide is added dropwise
Sodium water solution；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, the 15- of water and processing compound amount total weight
25% sodium hydroxide mixture；
The elution absorbing liquid is that the sodium hydroxide of the 15-25% of the water and processing compound amount total weight that are prepared by synthetic ratio is mixed
Close object.
5. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 4, it is characterised in that：Step
（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle is transferred to
In synthesis reactor, according to step in synthesis reactor（1）In proportioning bromine is added dropwise and while be passed through chlorine, a dropping step（1）In
The sodium hydroxide of the remaining 75%-85% of processing compound amount total weight, synthesizes bromochloroin again；Simultaneously in environmentally friendly absorption tower in
Elution absorbing liquid is transferred in tail gas absorption kettle and step is added（1）5, the 5- Dimethyl Hydan of synthetic ratio, as tail gas absorption
The tail gas absorption liquid of kettle uses；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
6. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 1, it is characterised in that：Step
（1）The middle synthetic method for preparing bromochloroin is routinely to match to generate 5,5- Dimethyl Hydan when producing C5H6Br2N2O2
The mother liquor containing sodium bromide in dissolve, use chlorine as halogenating agent, at the same be added dropwise mass fraction be 30-37% sodium hydroxides it is molten
Liquid carries out bromination and chlorination reaction；
The tail gas absorption liquid is the 5,5- Dimethyl Hydan prepared by synthetic ratio, mother liquor and processing compound containing sodium bromide
The mass fraction for measuring the 15-25% of total weight is the sodium hydroxide solution mixture of 30-37%；
The elution absorbing liquid is that the mass fraction of the water prepared by synthetic ratio and processing compound amount total weight 15-25% are 30-
37% sodium hydroxide solution mixture.
7. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 6, it is characterised in that：Production
The mother liquor containing sodium bromide generated when C5H6Br2N2O2 is：With 5,5- Dimethyl Hydan, sodium hydroxide, bromine for raw material, rub
You are than being 1：（2.0-2.1）：（2.0-2.2）, in aqueous solution, controlling reaction temperature is added dropwise bromine and carries out at -5 DEG C to 35 DEG C
Bromination reaction, after the completion of reaction, it is C5H6Br2N2O2 mother liquor that C5H6Br2N2O2, remaining liquid are removed in centrifugation.
8. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 6, it is characterised in that：Step
（2）In, work as step（1）In synthesis reactor complete batch materials synthesis, after empty kettle, the tail gas absorption liquid in tail gas absorption kettle is transferred to
In synthesis reactor, chlorine, while a dropping step are passed through in synthesis reactor（1）The middle remaining 75%-85%'s of processing compound amount total weight
Mass fraction is 30-37% sodium hydroxide solutions, synthesizes bromochloroin again；Elution absorbing liquid interior in environmentally friendly absorption tower simultaneously
It is transferred in tail gas absorption kettle and step is added（1）5, the 5- Dimethyl Hydan of synthetic ratio, the tail gas as tail gas absorption kettle are inhaled
Liquid is received to use；Elution absorbing liquid in environmentally friendly absorption tower is prepared again.
9. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 1, it is characterised in that：It is described
Tail gas absorption liquid pH value in tail gas absorption kettle is 12 or more；Feed temperature is at 5-15 DEG C in control tail gas absorption kettle.
10. the tail gas treatment process in a kind of bromochloroin building-up process according to claim 1, it is characterised in that：Institute
The elution absorbing liquid pH value in environmentally friendly absorption tower is stated 12 or more.
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