CN103468175B - Method for preparing paper tube adhesive through utilizing high-concentration printing, dyeing and desizing wastewater - Google Patents
Method for preparing paper tube adhesive through utilizing high-concentration printing, dyeing and desizing wastewater Download PDFInfo
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- CN103468175B CN103468175B CN201310355694.6A CN201310355694A CN103468175B CN 103468175 B CN103468175 B CN 103468175B CN 201310355694 A CN201310355694 A CN 201310355694A CN 103468175 B CN103468175 B CN 103468175B
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- 239000002351 wastewater Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000007639 printing Methods 0.000 title claims abstract description 27
- 238000009990 desizing Methods 0.000 title claims abstract description 25
- 239000000853 adhesive Substances 0.000 title claims abstract description 23
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 23
- 238000004043 dyeing Methods 0.000 title abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 5
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 97
- 239000004202 carbamide Substances 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 13
- 239000013530 defoamer Substances 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 2
- 230000008901 benefit Effects 0.000 abstract description 8
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002518 antifoaming agent Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 abstract 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 42
- 229920002451 polyvinyl alcohol Polymers 0.000 description 42
- 239000000243 solution Substances 0.000 description 14
- 230000008569 process Effects 0.000 description 8
- 230000035484 reaction time Effects 0.000 description 7
- 238000004064 recycling Methods 0.000 description 6
- 239000012528 membrane Substances 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- -1 polysiloxane Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000009992 mercerising Methods 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010784 textile waste Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
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- Paper (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a method for preparing a paper tube adhesive through utilizing high-concentration printing, dyeing and desizing wastewater. The method comprises the following steps: determining the PVA content in the high-concentration printing, dyeing and desizing wastewater, adding a proper amount of a PVA raw material into the wastewater according to the determined PVA content to make the PVA content in an obtained solution reach 7.0-10.0wt%, adding kaolin and an antifoaming agent, heating the above obtained solution under stirring to 85-95DEG C for completely dissolving the raw material, controlling the temperature in a range of 80-85DEG C, adding formaldehyde, reacting for a certain time, adding an aldehyde removing agent for a reaction, naturally cooling to 40DEG C, and discharging to obtain the paper tube adhesive. The method realizes the zero emission of desizing wastewater, realizes the waste recycle by utilizing the PVA raw material in the desizing wastewater to prepare the paper tube adhesive, can be widely used I the treatment of the high-concentration printing, dyeing and desizing wastewater, and has obvious social and environmental benefits; and compared with other paper tube adhesives, the paper tube adhesive prepared through the method has the advantages of decrease of the cost by about 30%, and good economic benefit.
Description
(1) technical field
The present invention relates to a kind of method utilizing high-concentration dye-printing desizing waste water to prepare paper tube adhesive, belong to the recycling to PVA in high-concentration dye-printing desizing waste water.
(2) background technology
Textile waste, mainly from dyeing and finishing workshop section, comprises destarch, boiling-off, bleaching, mercerising, dyeing, stamp and arrangement etc.Desized wastewater generally accounts for about 10 ~ 20% of waste water total amount, waste water is in alkalescence, pH value is about 12, main component is for containing polyvinyl alcohol (PVA) (polymerization degree is between 1700 ~ 1750) slurry, and due to the difference of technique, the difference of cloth, in desized wastewater, the PVA content difference opposite sex is very large, PVA content is generally 1 ~ 3%, high density desized wastewater PVA content can reach 4 ~ 5%, and waste water COD cr is at 15000 ~ 70000mg/L, and its COD lifting capacity can account for 50% of total amount in dyeing waste water.Meanwhile, because the existence of PVA, desized wastewater biochemical is very poor (B/C is about about 0.1) also.
At present, the main methods of printing and dyeing enterprise to desized wastewater has following several:
1, direct facture.A lot of enterprise is all direct at present mixes desized wastewater and other waste water, utilizes the existing treatment facility of enterprise to process.The method not only makes Enterprise Integrated waste water COD increase, and biochemical is deteriorated, and processing cost also large increase.
2, chemical coagulation method.PVA belongs to non-ionic type organic polymer, and the electric charge that general flocculation agent produces is more weak to its adsorption, does not almost have effect to the removal of PVA.But the PVA aqueous solution is when there being more salt, because salting out can make PVA separate out.There is enterprise to pass through in desized wastewater, add sodium sulfate and borax at present, carry out continuously coagulation treatment to PVA under certain condition, to realize the COD removed in F waste water and the object reclaiming PVA.The clearance of this method COD can reach about 80%.But the source of the PVA concentrated solution that the salinity obtained after reclaiming is higher often becomes a difficult problem for enterprise, current most enterprise adopts entrusts other enterprises to carry out burning disposal.
3, membrane processing method.Membrane separation technique is by reaching the object of purifying waste water to the separation concentration and recovery of Pollutants in Wastewater.Mainly contain micro-filtration ultrafiltration nanofiltration and reverse osmosis membrane, partition method has energy-conservation without advantages such as the easy equipment of phase change operation are simple, and can reclaim recycling material, and it is practicable for being proved in treatment of dyeing wastewater.Embrane method process desized wastewater, COD clearance can reach 60-90%, but when processing desized wastewater, need in film treating processes to regularly replace membrane module, working cost is higher, and, concentrated solution after film process is for most printing and dyeing enterprise, or the problem of a headache.
Therefore, for printing and dyeing enterprise, if can process desized wastewater taking effective means, can remove the COD in waste water, can carry out recycling to the main raw material PVA in desized wastewater again, environmental benefit and economic benefit will be very remarkable.
(3) summary of the invention
The object of the invention is PVA in recycling treatment high-concentration dye-printing desizing waste water, provide a kind of method utilizing high-concentration dye-printing desizing waste water to prepare paper tube adhesive.
The technical solution used in the present invention is:
Utilize high-concentration dye-printing desizing waste water to prepare a method for paper tube adhesive, described method comprises following sequential steps:
(1) get high-concentration dye-printing desizing waste water, the content of PVA in wastewater measurement, the PVA content according to measuring adds appropriate PVA raw material (consistent with the PVA polymerization degree in waste water) again, makes PVA content in solution reach 7.0 ~ 10.0wt%; In described mensuration high-concentration dye-printing desizing waste water, the method for the content of PVA can be spectrophotometry; High density desized wastewater PVA content is generally 3 ~ 5wt%;
(2), after adding kaolin and defoamer, adjust pH, under 1.0 ~ 2.0,100 ~ 200r/min speed stir, solution is heated to 85 ~ 95 DEG C, raw material is dissolved completely; The ratio of described high-concentration dye-printing desizing waste water, kaolin, defoamer consumption is 1000mL:200 ~ 500g:5 ~ 20g; Described defoamer is this area conventional antifoam, comprise polysiloxane, polyethers, silicon and ether grafting, containing amine, imines and amides etc.;
(3) control temperature is at 80 ~ 85 DEG C, adds formaldehyde reaction 60 ~ 90min, and the ratio of described high-concentration dye-printing desizing waste water, formaldehyde consumption is 1000mL:5 ~ 40g; In formaldehyde and waste water, PVA mass ratio is advisable between 0.1 ~ 0.3.
This step is PVA acetalation.Its chemical reaction mechanism is shown below:
(4) naturally cool to 40 DEG C of dischargings, obtain described paper tube adhesive.
Preferably, be the free formaldehyde removed in product, add after formaldehyde reaction terminates in step (3), first add ammoniacal liquor regulator solution pH value to 7.0 ~ 8.0, then add urea, after 80 ~ 85 DEG C of insulation reaction 40 ~ 60min, carry out the operation of step (4) again; The ratio of described high-concentration dye-printing desizing waste water, amount of urea is 1000mL:1 ~ 10g.In urea and waste water, PVA mass ratio is advisable between 0.5 ~ 1.0.
This step is urea aldehyde reaction, and object removes free formaldehyde.Its chemical reaction mechanism is as follows:
The inventive method is from Green Chemistry changing waste into resources theory, not only achieve " zero " discharge of dye-printing desizing waste water, especially with high density desized wastewater for raw material, utilize high density desized wastewater to prepare paper tube adhesive, thus really reach the harmonious development of environment and'economy.
Beneficial effect of the present invention is: the method not only achieves " zero " discharge of desized wastewater, and paper tube adhesive prepared by the PVA raw material that make use of in desized wastewater, achieve the recycling treatment of refuse, the process of high-concentration dye-printing desizing waste water can be widely used in, there is significantly society and environmental benefit; And the paper tube adhesive that present method prepares is compared with other paper tube glues, cost is low by about 30%, has good economic benefit.
(4) accompanying drawing explanation
Fig. 1 recycling treatment high-concentration dye-printing desizing waste water prepares the process flow sheet of paper tube adhesive;
The relation in Fig. 2 free formaldehyde content and reaction times;
Fig. 3 formaldehyde and PVA add the relation of mass ratio and free formaldehyde content;
Fig. 4 urea and PVA add the relation of mass ratio and free formaldehyde.
(5) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
Present invention process schema is see Fig. 1, and concrete steps are as follows:
The high density desized wastewater (Shaoxing printing and dyeing mill embroidery cloth desized wastewater) of A, 1000ml, to record PVA content be the 3.80wt%(polymerization degree is 1700), be poured in the there-necked flask of 2L, add the PVA raw material 42.0g consistent with the PVA polymerization degree in waste water, make solution PVA content be about 8.0wt%.
B, add 260g kaolin and 9g defoamer (is purchased from defoamer company limited of Nanjing Huaxing, model XPK-20, for polysiloxane type defoamer), and add 1mol/L HCl solution, solution ph is adjusted to 2.0, then solution is heated to 95 DEG C, and stirs with agitator, stirring velocity is 100r/min, and the material such as PVA, kaolin is dissolved completely.
C, after PVA, kaolin dissolve completely, adjustment heating instrument, temperature of reaction system is controlled at 80 ~ 85 DEG C, and adds formaldehyde (HCHO) 16g, reaction 60min, after formaldehyde and PVA react completely, naturally cool to 40 DEG C of dischargings, obtain described paper tube adhesive product.
Embodiment 2:
Reaction conditions is with embodiment 1, and difference is, after C adds formaldehyde, the reaction times is 20min, and other operations and condition are with embodiment 1.
Embodiment 3:
Reaction conditions is with embodiment 1, and difference is, after C adds formaldehyde, the reaction times is 30min, and other operations and condition are with embodiment 1.
Embodiment 4:
Reaction conditions is with embodiment 1, and difference is, after C adds formaldehyde, the reaction times is 40min, and other operations and condition are with embodiment 1.
Embodiment 5:
Reaction conditions is with embodiment 1, and difference is, after C adds formaldehyde, the reaction times is 90min, and other operations and condition are with embodiment 1.
The relation of embodiment 2 ~ 5 differential responses time and free formaldehyde content is see Fig. 2; As seen from the figure, the reaction times, free formaldehyde content was less when more than 60min, and therefore the step C reaction times is preferably 60 ~ 90min.
Embodiment 6:
Reaction conditions is with embodiment 1, and difference is, it is 8g that C adds formaldehyde (HCHO), and other operations and condition are with embodiment 1.
Embodiment 7:
Reaction conditions is with embodiment 1, and difference is, it is 24g that C adds formaldehyde (HCHO), and other operations and condition are with embodiment 1.
Embodiment 8:
Reaction conditions is with embodiment 1, and difference is, it is 32g that C adds formaldehyde (HCHO), and other operations and condition are with embodiment 1.
The relation of the different formaldehyde add-on of embodiment 1 and 6 ~ 8 and free formaldehyde content is see Fig. 3, and as seen from the figure, formaldehyde add-on larger (i.e. formaldehyde/PVA ratio is larger), free formaldehyde content is larger.
Embodiment 9:
Reaction conditions is with embodiment 1, and difference is, after formaldehyde and PVA react completely in C, then adds ammoniacal liquor, regulator solution pH value to 7.0, and adds urea 2g, insulation reaction 50min, then naturally cools to 40 DEG C of dischargings, obtains described paper tube adhesive product.
Embodiment 10:
Reaction conditions is with embodiment 1, and difference is, after formaldehyde and PVA react completely in C, then adds ammoniacal liquor, regulator solution pH value to 7.0, and adds urea 4g, insulation reaction 50min, then naturally cools to 40 DEG C of dischargings, obtains described paper tube adhesive product.
Embodiment 11:
Reaction conditions is with embodiment 1, and difference is, after formaldehyde and PVA react completely in C, then adds ammoniacal liquor, regulator solution pH value to 7.0, and adds urea 6g, insulation reaction 50min, then naturally cools to 40 DEG C of dischargings, obtains described paper tube adhesive product.
Embodiment 12:
Reaction conditions is with embodiment 1, and difference is, after formaldehyde and PVA react completely in C, then adds ammoniacal liquor, regulator solution pH value to 7.0, and adds urea 8g, insulation reaction 50min, then naturally cools to 40 DEG C of dischargings, obtains described paper tube adhesive product.
The relation of the different urea addition of embodiment 9 ~ 12 and free formaldehyde content is see Fig. 4; As seen from the figure, urea add-on larger (i.e. urea/PVA ratio is larger), free formaldehyde content is less.
Prepare product according to the inspection of relevant analytical procedure, indices all can reach the requirement of salable product in paper tube glue industry standard at optimum conditions.
The concrete assay of embodiment 10 ~ 12, as following table, illustrates that, under the processing condition that embodiment 10 ~ 12 is such, the product obtained can reach the technical indicator of paper tube adhesive substantially.
Claims (2)
1. utilize high-concentration dye-printing desizing waste water to prepare a method for paper tube adhesive, described method comprises following sequential steps:
(1) get high-concentration dye-printing desizing waste water, the content of PVA in wastewater measurement, the PVA content according to measuring adds appropriate PVA raw material, makes PVA content in solution reach 7.0 ~ 10.0wt%;
(2), after adding kaolin and defoamer, adjust pH, under 1.0 ~ 2.0,100 ~ 200r/min speed stir, solution is heated to 85 ~ 95 DEG C, raw material is dissolved completely; The ratio of described high-concentration dye-printing desizing waste water, kaolin, defoamer consumption is 1000mL:200 ~ 500g:5 ~ 20g;
(3) control temperature is at 80 ~ 85 DEG C, adds formaldehyde reaction 60 ~ 90min, and the ratio of described high-concentration dye-printing desizing waste water, formaldehyde consumption is 1000mL:5 ~ 40g;
(4) naturally cool to 40 DEG C of dischargings, obtain described paper tube adhesive.
2. the method for claim 1, after it is characterized in that adding formaldehyde reaction in step (3) terminates, first add ammoniacal liquor regulator solution pH value to 7.0 ~ 8.0, then add urea, after 80 ~ 85 DEG C of insulation reaction 40 ~ 60min, carry out the operation of step (4) again; The ratio of described high-concentration dye-printing desizing waste water, amount of urea is 1000mL:1 ~ 10g.
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| CN201310355694.6A CN103468175B (en) | 2013-08-15 | 2013-08-15 | Method for preparing paper tube adhesive through utilizing high-concentration printing, dyeing and desizing wastewater |
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| CN201310355694.6A CN103468175B (en) | 2013-08-15 | 2013-08-15 | Method for preparing paper tube adhesive through utilizing high-concentration printing, dyeing and desizing wastewater |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105670538A (en) * | 2016-03-28 | 2016-06-15 | 广西金虹环保包装科技有限公司 | Preparation method of adhesive for paper tubes |
| CN109080286A (en) * | 2018-07-23 | 2018-12-25 | 佛山市品格包装材料有限公司 | Water transfers workpiece polyvinyl alcohol residual layer treatment fluid and processing method |
| CN109535285B (en) * | 2018-12-20 | 2021-06-01 | 深圳市星河环境技术有限公司 | Resource utilization method and system for PVA waste adhesive |
| CN114316849A (en) * | 2021-12-31 | 2022-04-12 | 沈光强 | Method for preparing paper tube adhesive from printing and dyeing wastewater |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962795A (en) * | 2005-11-07 | 2007-05-16 | 吴志峰 | Wood adhesive made from wet-process fiber board waste water |
| CN102173493A (en) * | 2011-03-08 | 2011-09-07 | 北京市环境保护科学研究院 | Process for removing polyvinyl alcohol in waste water |
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| RU1790577C (en) * | 1991-06-26 | 1993-01-23 | Владимир Иванович Андропов | Method of producing of finely dispersed polymer filler |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1962795A (en) * | 2005-11-07 | 2007-05-16 | 吴志峰 | Wood adhesive made from wet-process fiber board waste water |
| CN102173493A (en) * | 2011-03-08 | 2011-09-07 | 北京市环境保护科学研究院 | Process for removing polyvinyl alcohol in waste water |
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