CN102503946A - Gas phase process decolorization method of methenamine mother liquor and decolorization device thereof - Google Patents
Gas phase process decolorization method of methenamine mother liquor and decolorization device thereof Download PDFInfo
- Publication number
- CN102503946A CN102503946A CN2011103010389A CN201110301038A CN102503946A CN 102503946 A CN102503946 A CN 102503946A CN 2011103010389 A CN2011103010389 A CN 2011103010389A CN 201110301038 A CN201110301038 A CN 201110301038A CN 102503946 A CN102503946 A CN 102503946A
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- CN
- China
- Prior art keywords
- mother liquor
- groove
- decolouring
- mother
- decolorization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012452 mother liquor Substances 0.000 title claims abstract description 151
- 238000000034 method Methods 0.000 title claims abstract description 43
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004042 decolorization Methods 0.000 title abstract 16
- 235000010299 hexamethylene tetramine Nutrition 0.000 title abstract 4
- 229960004011 methenamine Drugs 0.000 title abstract 4
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000010413 mother solution Substances 0.000 claims description 25
- 238000004064 recycling Methods 0.000 claims description 25
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 8
- 238000004062 sedimentation Methods 0.000 abstract 4
- 239000012071 phase Substances 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000007791 dehumidification Methods 0.000 description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 208000019932 Aciduria Diseases 0.000 description 1
- 241001270131 Agaricus moelleri Species 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 241000130764 Tinea Species 0.000 description 1
- 208000002474 Tinea Diseases 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 230000002070 germicidal effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 208000019206 urinary tract infection Diseases 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Landscapes
- Gas Separation By Absorption (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to the technical field of gas phase process production of methenamine and particularly relates to a gas phase process decolorization method of methenamine mother liquor and a decolorization device thereof. The decolorization device comprises a mother liquor circulation tank, a mother liquor decolorization tank, a plate and frame filter press and a mother liquor sedimentation tank, and the decolorization method comprises the following steps: sending the methenamine mother liquor to be decolorized into the mother liquor decolorization tank, adding activated carbon into the mother liquor decolorization tank to adsorb impurities, driving into the plate and frame filter press to filter the activated carbon after the impurities are adsorbed by the activated carbon, enabling the mother liquor after filtration to enter into the mother liquor sedimentation tank, removing the impurities and the activated carbon in the mother liquor in the mother liquor sedimentation tank via a sedimentation role, enabling clear liquid of the mother liquor to flow back to the mother liquor decolorization tank for circulating decolorization till the decolorization of the mother liquor is qualified, enabling the mother liquor with the qualified decolorization to flow into the mother liquor circulation tank, and enabling the mother liquor to re-enter into an ammoniation reactor to react through the mother liquor circulation tank. The decolorization method and the decolorization device, disclosed by the invention, have the beneficial effects that the quality of a product is improved after decolorization treatment.
Description
Technical field
The present invention relates to the urotropine by using gas phase method production technical field, particularly a kind of decoloring method of urotropine by using gas phase method mother liquor and decoloring equipment thereof.
Background technology
Urotropine is as resin and the solidifying agent of plastics, the vulcanization accelerator (vulkacit H) of rubber, the sanforzing agent of textiles, and is used to make sterilant, explosive etc.When medicinal, back for oral administration is met the aciduria decomposition and is produced formaldehyde and play germicidal action, is used for slight urinary tract infections; Be used to outward control tinea, hidroschesis, control underarm odor.Mix with caustic soda and sodium phenylate, be used for smoke mask and make the phosgene absorption agent.Urotropine still is a kind of inhibiter commonly used, is used to slow down Corrosion of Metallic Materials.
Vapor phase process prepares in the urotropine process, but the equipment of producing urotropine is after operation for some time, because the existence of formic acid in the formaldehyde.Mist of oil carries that reason can generate the brown polymkeric substance of thickness with temperature of reaction is higher etc. secretly in the gas ammonia.These resultants can influence urotropine outward appearance, purity and ash content.
Summary of the invention
The technical problem that the present invention will solve is: a kind of decoloring method and decoloring equipment thereof of urotropine by using gas phase method mother liquor are provided, can be at set intervals to the processing of decolouring of urotropine mother liquor.
The technical solution adopted for the present invention to solve the technical problems is: a kind of decoloring method of urotropine by using gas phase method mother liquor, with the urotropine mother liquor of needs decolouring, send into mother liquor decolouring groove; In mother liquor decolouring groove, add gac and carry out impurity absorption; Behind charcoal absorption impurity, to squeeze into plate-and-frame filter press and filter gac wherein, the mother liquor after the filtration gets into the mother liquor settling bath; Impurity in the mother liquor and gac are removed through settlement action in the mother liquor settling bath; The mother liquor clear liquid flows back to mother liquor decolouring groove circulation decolouring, and qualified until the mother liquor decolouring, the qualified mother liquor that decolours is returned ammoniation reactor and reacted again.
Further, the mother liquor clear liquid overflows back mother liquor decolouring groove through the mode of overflow, and the mother liquor that decolours qualified flows into the Recycling Mother Solution groove, gets into ammoniation reactor again through the Recycling Mother Solution groove and reacts.
Further, the add-on of gac is 20～50% of a mother liquor, and heating absorption impurity, keeps interior temperature 70-80 ℃ of mother liquor decolouring groove.
Further, gac is the gac of powdery alkalescence.
A kind of decoloring equipment of urotropine by using gas phase method mother liquor; Comprise Recycling Mother Solution groove, mother liquor decolouring groove, plate-and-frame filter press and mother liquor settling bath; The Recycling Mother Solution groove respectively with mother liquor decolouring groove, urotropine by using gas phase method preparation facilities in the mother liquor outlet be connected with ammoniation reactor; To squeeze into mother liquor decolouring groove through the mother liquor of mother liquor outlet inflow Recycling Mother Solution groove decolours; And the qualified mother liquor that will decolour squeezes into ammoniation reactor, and mother liquor decolouring groove, plate-and-frame filter press circulate successively with the mother liquor settling bath and be connected, mother liquor the to be decoloured decolouring that in mother liquor decolours groove, plate-and-frame filter press and mother liquor settling bath, circulates; The mother liquor settling bath is connected with the Recycling Mother Solution groove, and the qualified mother liquor of decolouring is returned the Recycling Mother Solution groove.
Particularly, mother liquor decolouring groove is the storage tank of band heating coil.
Particularly, the crystallization groove in Recycling Mother Solution groove and the urotropine by using gas phase method preparation facilities is connected with mother liquor outlet on the whizzer.
The invention has the beneficial effects as follows: after handling through decolouring of the present invention, improved the quality of product.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is a structure diagram of the present invention;
Among the figure 1, ammoniation reactor, 2, the crystallization groove, 3, whizzer, 4, dehumidification system; 5, reclaim washing tower, 6, ammonia absorber, 7, condensing surface, 8, dashpot; 9, tail gas absorber, 10, Analytic Tower, 11, plate-and-frame filter press, 12, the mother liquor settling bath; 13, Recycling Mother Solution groove, 14, mother liquor decolouring groove, 15, mother liquor decolouring pump, 16, recycle pump.
Embodiment
A kind of urotropine by using gas phase method as shown in Figure 1 prepares equipment, has ammoniation reactor 1, and the material outlet place, lower end of ammoniation reactor 1 is connected with crystallization groove 2; Be connected with whizzer 3 on the crystallization groove 2, be connected with dehumidification system 4 on the whizzer 3, dehumidification system 4 upper ends are connected with reclaims washing tower 5; The upper end of ammoniation reactor 1 is connected with ammonia absorber 6; The upper end of ammonia absorber 6 is connected with condensing surface 7, and the bottom of condensing surface 7 is connected with dashpot 8, and the upper end of dashpot 8 is connected with tail gas absorber 9; The top of ammoniation reactor 1 is connected with Analytic Tower 10, and the bottom of Analytic Tower 10 is connected the lower end of ammonia absorber 6, condensing surface 7 and dashpot 8.
As shown in Figure 1; Prepare the decoloring equipment that increases by a cover urotropine by using gas phase method mother liquor in the equipment at this urotropine by using gas phase method; Can be at set intervals to the processing of decolouring of urotropine mother liquor; Improve the quality of product, this decoloring equipment comprises Recycling Mother Solution groove 13, mother liquor decolouring groove 14, plate-and-frame filter press 11 and mother liquor settling bath 12, Recycling Mother Solution groove 13 respectively with mother liquor decolouring groove 14, urotropine by using gas phase method preparation facilities in the mother liquor outlet be connected with ammoniation reactor 1; To squeeze into mother liquor decolouring groove 14 through the mother liquor of mother liquor outlet inflow Recycling Mother Solution groove 13 decolours; And the qualified mother liquor that will decolour squeezes into ammoniation reactor 1, and mother liquor decolouring groove 14, plate-and-frame filter press 11 circulates successively with mother liquor settling bath 12 and be connected, and mother liquor to be decoloured circulates in mother liquor decolouring groove 14, plate-and-frame filter press 11 and mother liquor settling bath 12 and decolours; Mother liquor settling bath 12 is connected with Recycling Mother Solution groove 13, and the qualified mother liquor of decolouring is returned Recycling Mother Solution groove 13.Particularly, the crystallization groove 2 in Recycling Mother Solution groove 13 and the urotropine by using gas phase method preparation facilities is connected with mother liquor outlet on the whizzer 3.
A kind of decoloring method of urotropine by using gas phase method mother liquor; With the urotropine mother liquor of needs decolouring, send into mother liquor decolouring groove 14, mother liquor decolouring groove 14 flat-top flat cover cylindrical tanks for the band heating coil; Be provided with in the storage tank and mark time, so that the cleaning of mother liquor decolouring groove 14.In mother liquor decolouring groove 14, add the gac of a certain amount of powdery alkalescence, the add-on of gac is 2～5% of a mother liquor, and heating absorption impurity, and mother liquor decolouring groove 14 needs same steam insulation, in general normal running needs temperature 70-80 ℃.
Mother liquor in the mother liquor decolouring groove 14 decolours through mother liquor, and pump 15 is squeezed into plate-and-frame filter press 11, mother liquor settling bath 12 loops back and flows into mother liquor decolouring groove 14, and the reflux time looks the mother liquor shade and decides, and is generally 30～45min, specifically is as the criterion with mother liquor discharging color.Mother liquor decolouring groove 14 is provided with the internal heating coil pipe, and heating coil feeds steam to guarantee the temperature of absorption.
Behind charcoal absorption impurity, squeeze into plate-and-frame filter press 11 with mother liquor decolouring pump 15.When just beginning,, discharge the mother liquor black in color probably because filter cake does not form.Therefore still flow back to mother liquor decolouring groove 14.Send into mother liquor settling bath 12 when mother liquor is after faint yellow, mother liquor settling bath 12 is a pyramidal structure suspension type storage tank for the bottom, and impurity in the mother liquor and gac are removed through settlement action at the mother liquor settling bath.The riser of also underproof mother liquor clear liquid through mother liquor settling bath 12 that decolour overflows back mother liquor decolouring groove.The mother liquor that decolours qualified flows into Recycling Mother Solution groove 13, and the qualified mother liquor in the Recycling Mother Solution groove 13 is squeezed into ammoniation reactor 1 through recycle pump 16 with mother liquor and reacted.
The mother liquor decolouring is operating as intermittent operation, if mother liquor is settled solution in the normal productive process, can decolour, and directly gets into next process and gets final product.The decolouring operation will be paid special attention to not remain in gac in the mother liquor, in order to avoid influence the urotropine quality.
Claims (7)
1. the decoloring method of a urotropine by using gas phase method mother liquor is characterized in that: the urotropine mother liquor that will decolour, send into mother liquor decolouring groove (14); In mother liquor decolouring groove (14), add gac and carry out impurity absorption; Behind charcoal absorption impurity, to squeeze into plate-and-frame filter press (11) and filter gac wherein, the mother liquor after the filtration gets into mother liquor settling bath (12); Impurity in the mother liquor and gac are removed through settlement action in mother liquor settling bath (12); The mother liquor clear liquid flows back to mother liquor decolouring groove (14) circulation decolouring, and qualified until the mother liquor decolouring, the qualified mother liquor that decolours is returned ammoniation reactor (1) and reacted again.
2. the decoloring method of urotropine by using gas phase method mother liquor according to claim 1; It is characterized in that: the mother liquor clear liquid overflows back mother liquor decolouring groove (14) through the mode of overflow; The mother liquor that decolours qualified flows into Recycling Mother Solution groove (13), gets into ammoniation reactor (1) again through Recycling Mother Solution groove (13) and reacts.
3. the decoloring method of urotropine by using gas phase method mother liquor according to claim 1 is characterized in that: the add-on of gac is 20～50% of a mother liquor, and heating absorption impurity, keeps interior temperature 70-80 ℃ of mother liquor decolouring groove (14).
4. the decoloring method of urotropine by using gas phase method mother liquor according to claim 1 is characterized in that: gac is the gac of powdery alkalescence.
5. the decoloring equipment of a urotropine by using gas phase method mother liquor; It is characterized in that: comprise Recycling Mother Solution groove (13), mother liquor decolouring groove (14), plate-and-frame filter press (11) and mother liquor settling bath (12); Recycling Mother Solution groove (13) respectively with mother liquor decolouring groove (14), urotropine by using gas phase method preparation facilities in the mother liquor outlet be connected with ammoniation reactor (1); To squeeze into mother liquor decolouring groove (14) through the mother liquor of mother liquor outlet inflow Recycling Mother Solution groove (13) decolours; And the qualified mother liquor that will decolour is squeezed into ammoniation reactor (1); Mother liquor decolouring groove (14), plate-and-frame filter press (11) circulate successively with mother liquor settling bath (12) and are connected; Mother liquor the to be decoloured decolouring that in mother liquor decolours groove (14), plate-and-frame filter press (11) and mother liquor settling bath (12), circulates, mother liquor settling bath (12) is connected with Recycling Mother Solution groove (13), and the qualified mother liquor of decolouring is returned Recycling Mother Solution groove (13).
6. the decoloring equipment of urotropine by using gas phase method mother liquor according to claim 5 is characterized in that: described mother liquor decolouring groove (14) is the storage tank of band heating coil.
7. according to the decoloring equipment of claim 5 or 6 described urotropine by using gas phase method mother liquors, it is characterized in that: the crystallization groove (2) in described Recycling Mother Solution groove (13) and the urotropine by using gas phase method preparation facilities is connected with mother liquor outlet on the whizzer (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110301038.9A CN102503946B (en) | 2011-09-30 | 2011-09-30 | Gas phase process decolorization method of methenamine mother liquor and decolorization device thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110301038.9A CN102503946B (en) | 2011-09-30 | 2011-09-30 | Gas phase process decolorization method of methenamine mother liquor and decolorization device thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102503946A true CN102503946A (en) | 2012-06-20 |
| CN102503946B CN102503946B (en) | 2014-06-18 |
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| CN201110301038.9A Active CN102503946B (en) | 2011-09-30 | 2011-09-30 | Gas phase process decolorization method of methenamine mother liquor and decolorization device thereof |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3753895A (en) * | 1971-04-19 | 1973-08-21 | Texaco Inc | Separation process for high carbon number straight chain hydrocarbonsby adsorption |
| US5346622A (en) * | 1993-03-04 | 1994-09-13 | Hewlett-Packard Company | Hydrocarbon class separation and quantitation by split column effluent analysis |
| CN1259518A (en) * | 1999-01-05 | 2000-07-12 | 曹官岐 | Prodn. technology of urotropine by ammoniation of formaldehyde |
| CN201686637U (en) * | 2010-04-01 | 2010-12-29 | 江苏恒茂机械制造有限公司 | Hexamethylenetetramine preparing device by gas phase method |
| CN102464662A (en) * | 2010-11-10 | 2012-05-23 | 孟宪新 | Novel system for urotropine mother liquor decoloration and filtration |
| CN202246493U (en) * | 2011-09-30 | 2012-05-30 | 江苏恒茂机械制造有限公司 | Device for decoloring urotropin mother liquor by using gas phase method |
-
2011
- 2011-09-30 CN CN201110301038.9A patent/CN102503946B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3753895A (en) * | 1971-04-19 | 1973-08-21 | Texaco Inc | Separation process for high carbon number straight chain hydrocarbonsby adsorption |
| US5346622A (en) * | 1993-03-04 | 1994-09-13 | Hewlett-Packard Company | Hydrocarbon class separation and quantitation by split column effluent analysis |
| CN1259518A (en) * | 1999-01-05 | 2000-07-12 | 曹官岐 | Prodn. technology of urotropine by ammoniation of formaldehyde |
| CN201686637U (en) * | 2010-04-01 | 2010-12-29 | 江苏恒茂机械制造有限公司 | Hexamethylenetetramine preparing device by gas phase method |
| CN102464662A (en) * | 2010-11-10 | 2012-05-23 | 孟宪新 | Novel system for urotropine mother liquor decoloration and filtration |
| CN202246493U (en) * | 2011-09-30 | 2012-05-30 | 江苏恒茂机械制造有限公司 | Device for decoloring urotropin mother liquor by using gas phase method |
Non-Patent Citations (3)
| Title |
|---|
| MARVIN J. FISHMAN，等: "Water analysis", 《ANALYTICAL CHEMISTRY》, vol. 41, no. 5, 30 April 1969 (1969-04-30), pages 323 - 360 * |
| 于兴辉: "10 kt/ a 乌洛托品装置工艺运行小结", 《中氮肥》, no. 3, 15 May 2007 (2007-05-15) * |
| 李广林: "乌洛托品及其生产方法", 《化肥工业》, vol. 24, no. 4, 28 August 1997 (1997-08-28) * |
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| CN102503946B (en) | 2014-06-18 |
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