CN101497617B - Method for producing hexamethylene tetramin by formaldehyde-containing wastewater - Google Patents
Method for producing hexamethylene tetramin by formaldehyde-containing wastewater Download PDFInfo
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- CN101497617B CN101497617B CN2009100967663A CN200910096766A CN101497617B CN 101497617 B CN101497617 B CN 101497617B CN 2009100967663 A CN2009100967663 A CN 2009100967663A CN 200910096766 A CN200910096766 A CN 200910096766A CN 101497617 B CN101497617 B CN 101497617B
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Abstract
The invention relates to a method for producing urotropine by utilizing wastewater containing formaldehyde. Ammonia is added into the wastewater containing the formaldehyde, and the mixture is stirred to react for 3 to 15 hours to obtain a dilute solution of the urotropine under the condition that the pH value is controlled to be between 7 and 12 and the reaction temperature is between 10 and 90 DEG C; one or more devices of a filter press, a bag filter and a precision filter are adopted to remove solid components of the dilute solution of the urotropine, then an activated carbon filter is used to remove a viscous liquid of the dilute solution of the urotropine, then a microporous filter membrane with a pore diameter of between 0.2 and 1mu m is used to remove micron and submicron impurities and floccules in the solution, an ultrafiltration membrane is used to remove soluble macromolecular impurities, and the pollution index of the solution is less than or equal to 5; and the treated solution enters a first-order film for separation, a first-order thin solution is directly discharged or is used for industrial circulating water, a first-order thick solution is collected and stored in a tank when the mass fraction of the urotropine in the first-order thick solution is more than or equal to 6 percent, the first-order thick solution enters a second-order film for the separation, a second-order thin solution returns to the first-order film for the separation, and a second-order thick solution is collected and stored in the tank when the mass fraction of the urotropine in the second-order thick solution reaches more than 10 percent.
Description
Technical field
The present invention relates to a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine, belong to waste water reclamation and utilize treatment process to make the field.
Background technology
Formaldehyde is a kind of important chemical material, agricultural chemicals, resin, etc. the field all use in a large number, contain a large amount of formaldehyde in a lot of agricultural chemicals, the waste water of chemical industry, simultaneously formaldehyde is that country's issue toxic substance is preferentially controlled on the register second, and therefore the pollution that is caused by formaldehyde waste water must strict control.
The massfraction of formaldehyde is generally below 5% in the present formaldehyde-containing wastewater, conventional method is difficult to reclaim, the general methods such as biochemistry, catalyzed oxidation, stripping that adopt are handled, but aforesaid method not only can not reclaim valuable formaldehyde, need to consume a large amount of energy and resource on the contrary, formaldehyde can not thoroughly be handled in the waste water simultaneously.
CN1196339A, title " production method of quick-acting urea-formaldehyde nitrogen fertilizer ", it is to add urea in formalin, the mole ratio that makes urea and formaldehyde is 2～5: 1, heating also keeps temperature of reaction at 70～90 ℃, after treating that urea all dissolves, cools off, add acid solution, make pH value 3～4, resultant of reaction promptly obtains quick-acting urea-formaldehyde nitrogen fertilizer after taking out drying, but can only utilize formaldehyde content in the formaldehyde solution more than 9%.
CN101070254A, title " a kind of method of utilizing formaldehyde waste water to ferment to produce fertilizer ", this method is carried out alkaline polymerization to the waste water that contains formaldehyde earlier, carries out the urea aldehyde reaction then, carries out catalyzed oxidation again, ferments at 50-70 ℃ at last.Its weak point: this method needs plurality of raw materials, treating processes loaded down with trivial details.
CN1259518A, title " ammoniation of formaldehyde system urotropine production technique ", it is to utilize useless formaldehyde through condensation reaction, vacuum concentration, drying and must the urotropine white crystal.Its weak point: not only require the content height of useless formaldehyde, and all obtain urotropine, need to consume a large amount of energy by evaporation concentration.
CN101328182A, title " utilize glyphosate waste water to produce hexamethylenetetramine and gyphosate solution method ", in the waste water of producing glyphosate, feed ammonia or add ammoniacal liquor, regulate the potential of hydrogen of waste water, make PH＞7, left standstill 6-13 hour, the glyphosate in the waste water, formaldehyde and ammonia react, then reaction solution is carried out evaporation concentration, crystallization filtration, obtaining filter cake is the hexamethylenetetramine runic, and runic is by dissolving, decolouring and recrystallization, and filtration drying makes the hexamethylenetetramine finished product; Filtrate with in the sulfuric acid and after make the gyphosate solution of sulfur-bearing ammonium.Its weak point: need steam heating, consumes energy.
Summary of the invention
Purpose of design: avoid the weak point in the background technology, design a kind of can either cutting down the consumption of energy effectively, can utilize the low levels formaldehyde waste water to produce the method for urotropine again.
Design: in order to realize above-mentioned purpose of design.The application adds ammonia and produces urotropine in formaldehyde-containing wastewater, utilize membrane technique to put forward the concentration of dense urotropine then, propose the production that urotropine solution after dense can be directly used in derived product, perhaps obtain the urotropine dry product, reach the combination that waste water treatment and resource reclaim through evaporation.
Technical scheme: utilize formaldehyde-containing wastewater to produce the method for urotropine, 1) in formaldehyde-containing wastewater, adds ammonia, between the control pH value 7～12,10～90 ℃ of following stirring reactions of temperature of reaction 3～15 hours, obtain the dilute solution of urotropine; 2) adopt one or more devices in pressure filter, bag type filtering machine, the accurate filter to remove the solids component of urotropine dilute solution, remove the viscous liquid of urotropine dilute solution again with activated charcoal filter, be impurity and the floss that the micropore filtering film of 0.2～1 μ m is removed micron, submicron in the solution with the aperture then, remove soluble large molecule impurity with ultra-filtration membrane, the pollution index of solution≤5; 3) solution after handling enters the one-level film and separates, the light liquid of one-level directly discharges or is used for industrial circulating water and uses, in the one-level dope massfraction of urotropine reach 〉=collected in 6% o'clock with storage tank in, the dense secondary film that enters of one-level separates, the light liquid of secondary is got back to the one-level film and is separated, in the secondary dope massfraction of urotropine reach 10% collect when above with storage tank in.
The present invention compares with background technology, and the one, the formaldehyde in the waste water can be any concentration, the formaldehyde in the waste water is utilized effectively, remarkable in economical benefits; The 2nd, the process of utilizing membrane technique to carry dense urotropine solution does not have phase transformation, need not steam, and energy-saving effect is obvious; The 3rd, carry the urotropine solution purity height after dense, can be directly used in the production of derived product; The 4th, the waste water noresidue formaldehyde after handling can directly discharge or apply mechanically as process water, really realizes zero release.
Embodiment
Embodiment 1: utilize formaldehyde-containing wastewater to produce the method for urotropine, 1) in formaldehyde-containing wastewater, adds ammonia, between the control pH value 7～12, between preferred 8～11, more preferably between 8～9,10～90 ℃ of following stirring reactions of temperature of reaction 1～15 hour, 20～70 ℃ of following stirring reactions of preferable reaction temperature 3～10 hours, more preferably 40～60 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 4～8 hours;
2) adopt one or more devices in pressure filter, bag type filtering machine, the accurate filter to remove the solids component of urotropine dilute solution, preferred accurate filter is removed the solids component of urotropine dilute solution, remove the viscous liquid of urotropine dilute solution again with activated charcoal filter, be impurity and the floss that the micropore filtering film of 0.2～1 μ m is removed micron, submicron in the solution with the aperture then, remove soluble large molecule impurity with ultra-filtration membrane, the pollution index of solution≤5;
3) solution after handling enters the one-level film and separates, and the light liquid of one-level directly discharges or is used for that industrial circulating water uses or production labor skill water, in the one-level dope massfraction of urotropine reach 6% collect when above and storage tank in; The one-level dope enters the secondary film to be separated, and the light liquid of secondary is got back to the one-level film and separated, in the secondary dope massfraction of urotropine reach 10% collect when above with storage tank in;
4) the urotropine solution of carrying after dense obtains the solid urotropine through evaporation, cooling, crystallization, centrifugal, oven dry.
5) propose the production that urotropine solution after dense can be directly used in derived product.
According to method provided by the invention, containing the ammonia that adds in the formaldehyde can be liquefied ammonia, ammonia or ammoniacal liquor, the reaction of formaldehyde and ammonia can be carried out in the encloses container that a band stirs, and also can carry out in not with the container of stirring at one, utilizes the ammonia that feeds to stir naturally.According to method provided by the invention, the control of pH value is as the criterion when finishing with reaction.
According to method provided by the invention, the filtration of urotropine dilute solution can (glyphosate waste water wherein contains formaldehyde 0.5%-5% according to different waste water; N-(phosphonomethyl) iminodiacetic acid wastewater contains formaldehyde 0.5-5%) water quality determines used filter plant, preferred accurate filter also can select several combinations of pressure filter, bag type filtering machine, accurate filter to filter.According to method provided by the invention, ultra-filtration membrane can be the film between 1000～100000 according to the component selection molecular weight cut-off of waste water.
According to method provided by the invention, the one-level film can be selected a kind of in nanofiltration membrane, the reverse osmosis membrane or combination for use according to the water quality of waste water, and the secondary film can be selected a kind of or combination in nanofiltration membrane, the reverse osmosis membrane for use according to the water quality of waste water.According to method provided by the invention, ultra-filtration membrane is hollow-fibre membrane, rolled film, board-like film and tubular membrane, and one-level film, secondary film are rolled film.
Embodiment 2: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 7,10 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 15 hours.
Embodiment 3: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 7.5,20 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 14 hours.
Embodiment 4: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 8,30 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 13 hours.
Embodiment 5: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 8.5,40 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 12 hours.
Embodiment 6: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 9,50 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 11 hours.
Embodiment 7: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 9.5,60 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 10 hours.
Embodiment 8: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 10,65 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 9 hours.
Embodiment 9: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 10.5,70 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 8 hours.
Embodiment 10: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 11,75 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 7 hours.
Embodiment 11: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 11.5,80 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 6 hours.
Embodiment 12: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 12,90 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 5 hours.
Embodiment 13: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 8,70 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 4 hours.
Embodiment 14: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 9,80 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 3 hours.
Embodiment 15: on the basis of embodiment 1, in formaldehyde-containing wastewater, add ammonia, and control pH value 10,90 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 2 hours.
Embodiment 16: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8.25,60 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 8 hours.
Embodiment 17: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8.5,55 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 7 hours.
Embodiment 18: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8.75,50 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 6 hours.
Embodiment 19: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 9,45 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 5 hours.
Embodiment 20: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 9,40 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 4 hours.
Embodiment 21: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8,70 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 10 hours.
Embodiment 22: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8.4,60 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 9 hours.
Embodiment 23: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 8.7,50 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 8 hours.
Embodiment 24: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 9,40 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 7 hours.
Embodiment 25: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 9.4,30 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 6 hours.
Embodiment 26: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 9.8,20 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 5 hours.
Embodiment 27: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 10.2,20 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 3 hours.
Embodiment 28: on the basis of embodiment 1, add ammonia in formaldehyde-containing wastewater, between the control pH value preferred 11,60 ℃ of following stirring reactions of temperature of reaction obtained the dilute solution of urotropine in 7 hours.
Embodiment 29: in the reaction vessel that to be 1.5% waste water 1000kg with formaldehyde content stir as for band, add liquefied ammonia 6kg, and 30～35 ℃ of stirring reactions of controlled temperature 4 hours, PH=8.5, reaction finishes.Be that the accurate filter of 5 μ m filters and to enter the more medium filter that gac is housed by the aperture then, fluid is the solution that millipore filter, the ultra-filtration membrane of 0.5 μ m obtains pollution index≤5 through the aperture once.
Above-mentioned solution obtains one-level dope 236kg and is collected in process tank through the one-level membrane sepn, and the massfraction of urotropine is 6.1% by analysis, and light liquid 764 is collected in the water tank as process water; One-level dope 236kg obtains secondary dope 60kg and is collected in another process tank through the secondary membrane sepn, and the massfraction of urotropine is 24.25% by analysis, and light liquid 176kg turns back to one-level to be separated.
The massfraction of urotropine be 24.25% solution 60kg through the economic benefits and social benefits thickener concentrate, separation, drying, obtain the urotropine dry product of 11kg.The residue mother liquid recycle concentrates to following batch.
What need understand is: though the foregoing description is to the mentality of designing of the present invention detailed text description of contrasting; but these text descriptions; just the simple text of mentality of designing of the present invention is described; rather than to the restriction of mentality of designing of the present invention; any combination, increase or modification that does not exceed mentality of designing of the present invention all falls within the scope of protection of the present invention.
Claims (7)
1. method of utilizing formaldehyde-containing wastewater to produce urotropine is characterized in that:
1) in formaldehyde-containing wastewater, adds ammonia, between the control pH value 7～12,10～90 ℃ of following stirring reactions of temperature of reaction 3～15 hours, obtain the dilute solution of urotropine;
2) adopt one or more devices in pressure filter, bag type filtering machine, the accurate filter to remove the solids component of urotropine dilute solution, remove the viscous liquid of urotropine dilute solution again with activated charcoal filter, be impurity and the floss that the micropore filtering film of 0.2～1 μ m is removed micron, submicron in the solution with the aperture then, remove soluble large molecule impurity with ultra-filtration membrane, the pollution index of solution≤5, ultra-filtration membrane molecular weight cut-off are 1000～100000;
3) solution after handling enters the one-level film and separates, the light liquid of one-level directly discharges or is used for industrial circulating water and uses, the massfraction of urotropine reaches 〉=was collected in the storage tank in 6% o'clock in the one-level dope, the one-level dope enters the secondary film to be separated, the light liquid of secondary is got back to the one-level film and is separated, the massfraction of urotropine reaches at 10%～40% o'clock and is collected in the storage tank in the secondary dope, and the urotropine solution that massfraction reaches more than 10% obtains the solid urotropine through evaporation, cooling, crystallization, centrifugal, oven dry.
2. a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine according to claim 1, it is characterized in that: described ammonia is liquefied ammonia, ammonia, ammoniacal liquor.
3. a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine according to claim 1 is characterized in that: described control pH value 7～12,40～60 ℃ of following stirring reactions of temperature of reaction 4～8 hours.
4. a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine according to claim 1 is characterized in that: described one-level film is a kind of or combination in nanofiltration membrane, the reverse osmosis membrane, and described secondary film is a kind of or combination in nanofiltration membrane, the reverse osmosis membrane.
5. a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine according to claim 1, it is characterized in that: described ultra-filtration membrane is hollow-fibre membrane, rolled film, board-like film and tubular membrane.
6. according to claim 1 or 4 described a kind of methods of utilizing formaldehyde-containing wastewater to produce urotropine, it is characterized in that described one-level film, secondary film are rolled film.
7. a kind of method of utilizing formaldehyde-containing wastewater to produce urotropine according to claim 1 is characterized in that: the described one or more combination that is evaporated to single-effect evaporation, double-effect evaporation, multiple-effect evaporation.
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| CN102633314B (en) * | 2012-03-27 | 2014-07-09 | 江苏好收成韦恩农化股份有限公司 | Low-concentration formaldehyde wastewater resource recycling process |
| CN102746310B (en) * | 2012-07-06 | 2016-09-28 | 衡阳师范学院 | A kind of be raw material production industry hexamethylenamine with useless paraformaldehyde method |
| CN102992502A (en) * | 2012-11-15 | 2013-03-27 | 杭州天创环境科技股份有限公司 | Method for recovering low-concentration dimethylacetamide waste water |
| CN102993039A (en) * | 2012-12-18 | 2013-03-27 | 常州大学 | Method for recovering dimethyl acetamide in polyether sulfone spinning wastewater |
| CN103723864B (en) * | 2014-01-07 | 2016-01-27 | 杭州深瑞水务有限公司 | A kind for the treatment of process of ammonium chloride evaporative condensate |
| CN104387236B (en) * | 2014-09-29 | 2016-08-24 | 吴嘉 | A kind of propilolic alcohol, 1,4-butynediols and methenamine three coproduction continuous producing method |
| CN104672067A (en) * | 2014-12-12 | 2015-06-03 | 北京东方红升新能源应用技术研究院有限公司 | Method for refining polymethoxy dialkyl ether |
| CN105236608A (en) * | 2015-08-14 | 2016-01-13 | 苏州康博电路科技有限公司 | Method for directly applying wastewater to circulating water |
| CN110483530B (en) * | 2019-09-16 | 2021-10-12 | 山东泰和水处理科技股份有限公司 | Production method of urotropine for co-producing organic phosphine corrosion inhibitor |
| CN110790647A (en) * | 2019-11-19 | 2020-02-14 | 河北锦泰达化工有限公司 | Production system for preparing formaldehyde, paraformaldehyde, methylal and hexamethylenetetramine from methanol |
| CN110921996A (en) * | 2019-12-18 | 2020-03-27 | 水清华(天津)环保科技有限公司 | Glyphosate wastewater treatment method |
| CN111499031B (en) * | 2020-03-20 | 2022-08-16 | 广东粤海水务股份有限公司 | Nanofiltration method for purifying polluted shallow groundwater |
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