CN104004151A - Dicyandiamide-formaldehyde polymer and preparation method and applications thereof - Google Patents
Dicyandiamide-formaldehyde polymer and preparation method and applications thereof Download PDFInfo
- Publication number
- CN104004151A CN104004151A CN201410122985.5A CN201410122985A CN104004151A CN 104004151 A CN104004151 A CN 104004151A CN 201410122985 A CN201410122985 A CN 201410122985A CN 104004151 A CN104004151 A CN 104004151A
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- China
- Prior art keywords
- dyhard
- yuban
- formaldehyde
- preparation
- ammonium chloride
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920000642 polymer Polymers 0.000 title abstract 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000004043 dyeing Methods 0.000 claims description 8
- 238000004042 decolorization Methods 0.000 claims description 6
- 239000002351 wastewater Substances 0.000 claims description 6
- 239000008394 flocculating agent Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 19
- 239000007787 solid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention discloses a dicyandiamide-formaldehyde polymer and a preparation method and applications thereof. With the control of the molar ratio of dicyandiamide, ammonium chloride and formaldehyde between 0.52 to 0.60:0.56 to 0.64:1.2 to 1.8, the reaction temperature and the stirring speed, the usage amount of dicyandiamide is reduced and the dicyandiamide-formaldehyde polymer is produced. The method has characteristics of simple operation and low cost.
Description
Technical field
The present invention relates to a kind of polymkeric substance, relate in particular to a kind of preparation method and application thereof of Dyhard RU 100-yuban.
Background technology
It is that laking agent as in dyeing and printing auxiliary uses that Dyhard RU 100-yuban starts most, finds that afterwards it has the effect of coagulation reigning beauty.By many people Improvement, produced in a large number and for the processing of various dyeing waste waters, there is good decolouring and reduce the effect of COD, there is good using value.But because Dyhard RU 100 price is higher, cause its use cost higher, cause the difficulty of promoting the use of.In cyanamide-yuban synthetic method raw material used of improvement, except Dyhard RU 100, formaldehyde, ammonium chloride, also add the auxiliary agent such as urea or Tai-Ace S 150, attempted to reduce the usage quantity of Dyhard RU 100, reduced production costs.But effect not obvious, and add urea and under low temperature condition, easily occur even grumeleuse of layering blushing, add under Tai-Ace S 150 room temperature and there will be muddiness and layering, affect storage and the use of this polymkeric substance.
Application number is the synthetic method that 201010557601.4 Chinese patent " a kind of synthetic method of efficient printing and dying industry wastewater flocculating agent " discloses a kind of efficient printing and dying industry wastewater flocculating agent, and its Dyhard RU 100, ammonium chloride, the total mol ratio of formaldehyde are 0.8 ~ 1.5:1.6 ~ 2.8:2.9 ~ 4.0.This patent weak point is that the shared ratio of Dyhard RU 100 is still higher.
Application number is that 201210153455.8 Chinese patent " the liquid Dyhard RU 100 yuban of a kind of slant acidity and the application in dyeing industry thereof " discloses the liquid Dyhard RU 100 yuban of a kind of slant acidity, its components by weight percent is 20 ~ 24 parts of 100 parts of Dyhard RU 100s, mass concentration be 36% 65 ~ 68 parts of 158 ~ 162 parts of formalins, ammonium chlorides and the mass concentration inorganic acids that is 20%, this patent Dyhard RU 100 proportion nearly 1/3, higher, and cause cost high owing to also adding inorganic acid.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, preparation method and the application thereof of Dyhard RU 100-yuban that a kind of Dyhard RU 100 usage quantity is few, simple to operate, cost is low are provided.
Above-mentioned purpose of the present invention is achieved by following technical solution:
A kind of preparation method of Dyhard RU 100-yuban, adding formaldehyde limit toward limit in Dyhard RU 100 and ammonium chloride stirs, controlling temperature of reaction is 80 ~ 85 DEG C, and the mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.52 ~ 0.60:0.56 ~ 0.64:1.2 ~ 1.8, and described mixing speed is 50 ~ 100rpm.
Specifically comprise the steps:
S1. Dyhard RU 100 and ammonium chloride are put in reactor, then the stirring of formaldehyde limit is added on limit, stops heating while being heated to 45 DEG C simultaneously;
The mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.52 ~ 0.60:0.56 ~ 0.64:1.2 ~ 1.8, and described formaldehyde mass concentration is 38% ~ 42%, and described mixing speed is 50 ~ 100rpm;
S2. control temperature at 80 ~ 85 DEG C, react 2 ~ 3 hours, obtain Dyhard RU 100-yuban.
Further, first reactor is preheated to 35 ~ 45 DEG C before adding formaldehyde in described step S1.
Preferably, the mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.56:0.6:1.5.The present invention prepares the effective control to mixing speed and temperature in Dyhard RU 100-yuban process, makes reaction in optimum regime, has greatly improved reaction efficiency and the product quality of raw material, makes the consumption of Dyhard RU 100 few.
Further, first reactor is preheated to 35 ~ 45 DEG C before adding formaldehyde in described step S1.
Preferably, described mixing speed is 75 ~ 80rpm.
Further, the COD clearance of described Dyhard RU 100-yuban is more than 79%, and percent of decolourization is more than 95%.
Further, described Dyhard RU 100-yuban in dyeing industry as dye fixing agent; In dyeing industry as printing and dying industry wastewater flocculating agent.
Compared with prior art, beneficial effect of the present invention is as follows:
Technological operation is easy, realizes minimizing Dyhard RU 100 consumption by controlling mol ratio, temperature of reaction and the stirring velocity of Dyhard RU 100, ammonium chloride and formaldehyde, and production cost is lower, and product physico-chemical property is stable.
Embodiment
Below in conjunction with specific embodiment, the present invention is made further and being elaborated, but embodiment does not limit in any form the present invention.
Embodiment 1
In the there-necked flask with temperature-control device, add 0.52mol Dyhard RU 100,0.56mol ammonium chloride, the formaldehyde that is 38% by the 1.2mol mass concentration that is preheating to 40 DEG C slowly adds in flask, and stirs always, and stirring velocity is 50rpm; Finish, control temperature at 80 DEG C, reaction 2h, the colourless viscous liquid obtaining is Dyhard RU 100-yuban, recording solid content is 52.3%.
Embodiment 2
Except the molar weight of Dyhard RU 100, ammonium chloride and formaldehyde is respectively 0.6mol, 0.64mol, 1.8mol, other conditions are with embodiment 1;
Embodiment 3
Except stirring velocity is 100rpm, other conditions are with embodiment 1;
Embodiment 4
Except stirring velocity is 75rpm, other conditions are with embodiment 1;
Embodiment 5
Be 85 DEG C except controlling temperature of reaction, other conditions are with embodiment 1;
Comparative example 1
Except the molar weight of Dyhard RU 100, ammonium chloride and formaldehyde is respectively 0.51mol, 0.55mol, 1.1mol, other conditions are with embodiment 1;
Comparative example 2
Except the molar weight of Dyhard RU 100, ammonium chloride and formaldehyde is respectively 0.61mol, 0.65mol, 1.9mol, other conditions are with embodiment 1;
Comparative example 3
Except stirring velocity is 35rpm, other conditions are with embodiment 1;
Comparative example 4
Except stirring velocity is 105rpm, other conditions are with embodiment 1;
Comparative example 5
Be 75 DEG C except controlling temperature of reaction, other conditions are with embodiment 1;
Comparative example 6
Be 90 DEG C except controlling temperature of reaction, other conditions are with embodiment 1;
Get respectively 10 times of embodiment 1 ~ 5 and comparative example 1 ~ 6 samples with water dilutions, add respectively in the beaker that fills 1000mL dyeing waste water by the usage quantity of 100ppm, and stir 10 minutes, then leave standstill 8 hours, get supernatant liquor and measure respectively according to a conventional method colourity and COD.Result is as table 1:
| Project | The mol ratio of Dyhard RU 100, ammonium chloride and formaldehyde | Stirring velocity (rpm) | Reaction control temperature (DEG C) | Solid content (%) | COD clearance (%) | Percent of decolourization (%) |
| Embodiment 1 | 0.52：0.56：1.2 | 50 | 80 | 52.3 | 79.32 | 95.27 |
| Embodiment 2 | 0.6：0.64：1.8 | 50 | 80 | 56.2 | 82.56 | 96.12 |
| Embodiment 3 | 0.52：0.56：1.2 | 100 | 80 | 51.4 | 80.36 | 96.31 |
| Embodiment 4 | 0.52：0.56：1.2 | 75 | 80 | 52.8 | 83.14 | 95.84 |
| Embodiment 5 | 0.52：0.56：1.2 | 50 | 85 | 51.9 | 80.94 | 94.98 |
| Comparative example 1 | 0.51：0.55：1.1 | 50 | 80 | 51.9 | 78.21 | 90.78 |
| Comparative example 2 | 0.61：0.65：1.9 | 50 | 80 | 53.4 | 77.94 | 91.03 |
| Comparative example 3 | 0.52：0.56：1.2 | 35 | 80 | 49.7 | 74.23 | 89.87 |
| Comparative example 4 | 0.52：0.56：1.2 | 105 | 80 | 47.2 | 75.68 | 90.16 |
| Comparative example 5 | 0.52：0.56：1.2 | 50 | 75 | 51.1 | 78.53 | 90.86 |
| Comparative example 6 | 0.52：0.56：1.2 | 50 | 90 | 51.7 | 77.95 | 91.44 |
Can be obtained by upper table data, by embodiment 1,2 and comparative example 1,2 data contrast, comparative example 1,2 can solid content, COD clearance and percent of decolourization be all than embodiment 1,2 is low, and the mol ratio of Dyhard RU 100, ammonium chloride and formaldehyde is best in 0.52 ~ 0.60:0.56 ~ 0.64:1.2 ~ 1.8; By embodiment 1,3,4 contrast with the data of comparative example 3,4, only change this condition of stirring velocity, comparative example 3,4 can solid content, COD clearance and percent of decolourization be all than embodiment 1,3,4 is low, in preparation process, stirring velocity has certain influence to the present invention, and its scope 50 ~ 100rpm is optimum; Embodiment 1,5 is contrasted with the data of comparative example 5,6, only change temperature of reaction, comparative example 5,6 can solid content, COD clearance and percent of decolourization be all than embodiment 1,5 is low, and in preparation process, temperature of reaction has certain influence to the present invention, and its scope is 80 ~ 85 for best.
Claims (9)
1. the preparation method of a Dyhard RU 100-yuban, it is characterized in that, adding formaldehyde limit toward limit in Dyhard RU 100 and ammonium chloride stirs, controlling temperature of reaction is 80 ~ 85 DEG C, the mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.52 ~ 0.60:0.56 ~ 0.64:1.2 ~ 1.8, and described mixing speed is 50 ~ 100rpm.
2. the preparation method of Dyhard RU 100-yuban according to claim 1, is characterized in that, specifically comprises the steps:
S1. Dyhard RU 100 and ammonium chloride are put in reactor, then the stirring of formaldehyde limit is added on limit, stops heating while being heated to 45 DEG C simultaneously;
The mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.52 ~ 0.60:0.56 ~ 0.64:1.2 ~ 1.8, and described formaldehyde mass concentration is 38% ~ 42%, and described mixing speed is 50 ~ 100rpm;
S2. control temperature at 80 ~ 85 DEG C, react 2 ~ 3 hours, obtain Dyhard RU 100-yuban.
3. the preparation method of Dyhard RU 100-yuban according to claim 2, is characterized in that, adds the front reactor of formaldehyde and be first preheated to 35 ~ 45 DEG C in described step S1.
4. the preparation method of Dyhard RU 100-yuban according to claim 1 and 2, is characterized in that, the mol ratio of described Dyhard RU 100, ammonium chloride and formaldehyde is 0.56:0.6:1.5.
5. the preparation method of Dyhard RU 100-yuban according to claim 1 and 2, is characterized in that, described mixing speed is 75 ~ 80rpm.
6. prepare according to the preparation method of Dyhard RU 100-yuban described in claim 1 or 2 or 3 Dyhard RU 100-the yuban obtaining, it is characterized in that, the COD clearance of described Dyhard RU 100-yuban is more than 79%.
7. Dyhard RU 100-yuban according to claim 6, is characterized in that, the percent of decolourization of described Dyhard RU 100-yuban is more than 95%.
Dyhard RU 100-yuban according to claim 6 in dyeing industry as the application of dye fixing agent.
A Dyhard RU 100-yuban claimed in claim 6 in dyeing industry as the application of printing and dying industry wastewater flocculating agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410122985.5A CN104004151B (en) | 2014-03-31 | 2014-03-31 | A kind of preparation method and applications of dicandiamide-formaldehyde polymer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410122985.5A CN104004151B (en) | 2014-03-31 | 2014-03-31 | A kind of preparation method and applications of dicandiamide-formaldehyde polymer |
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| Publication Number | Publication Date |
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| CN104004151A true CN104004151A (en) | 2014-08-27 |
| CN104004151B CN104004151B (en) | 2016-08-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241992A (en) * | 2016-09-16 | 2016-12-21 | 淄博鲁瑞精细化工有限公司 | The preparation method of textile printing and dyeing wastewater decolorization flocculation agent |
| CN106883671A (en) * | 2017-03-29 | 2017-06-23 | 南宁市青秀区嘉利林化有限公司 | A kind of rosin ink color fixing agent and preparation method thereof |
| CN107720843A (en) * | 2017-10-31 | 2018-02-23 | 江苏工程职业技术学院 | A kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant |
| CN116618274A (en) * | 2023-06-05 | 2023-08-22 | 广州市一化数字科技有限公司 | PU motion terrace that possesses and keep solidification rate |
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| CN102476844A (en) * | 2010-11-23 | 2012-05-30 | 彭彦 | Synthetic method of efficient printing and dyeing wastewater flocculant |
| CN102895806A (en) * | 2012-10-17 | 2013-01-30 | 滁州市润达溶剂有限公司 | Coagulant and preparation method thereof |
| CN103351454A (en) * | 2013-07-01 | 2013-10-16 | 嘉兴学院 | Preparation method for modified dicyandiamide-formaldehyde flocculating agent and application of flocculating agent product |
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2014
- 2014-03-31 CN CN201410122985.5A patent/CN104004151B/en active Active
Patent Citations (5)
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| CN1607185A (en) * | 2003-10-15 | 2005-04-20 | 广东工业大学 | Production method of printing and dyeing wastewater coagulate decolourizer |
| CN102092830A (en) * | 2009-12-09 | 2011-06-15 | 上海康鸣高科技有限公司 | Method for producing coagulant for active dye wastewater |
| CN102476844A (en) * | 2010-11-23 | 2012-05-30 | 彭彦 | Synthetic method of efficient printing and dyeing wastewater flocculant |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241992A (en) * | 2016-09-16 | 2016-12-21 | 淄博鲁瑞精细化工有限公司 | The preparation method of textile printing and dyeing wastewater decolorization flocculation agent |
| CN106241992B (en) * | 2016-09-16 | 2019-01-29 | 淄博鲁瑞精细化工有限公司 | The preparation method of textile printing and dyeing wastewater decolorization flocculation agent |
| CN106883671A (en) * | 2017-03-29 | 2017-06-23 | 南宁市青秀区嘉利林化有限公司 | A kind of rosin ink color fixing agent and preparation method thereof |
| CN107720843A (en) * | 2017-10-31 | 2018-02-23 | 江苏工程职业技术学院 | A kind of synthesis technique of reactive dyed wastewater high-efficiency decolorant |
| CN116618274A (en) * | 2023-06-05 | 2023-08-22 | 广州市一化数字科技有限公司 | PU motion terrace that possesses and keep solidification rate |
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| CN104004151B (en) | 2016-08-17 |
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Effective date of registration: 20201125 Address after: 215000 Shengze Town, Wujiang District, Suzhou, Jiangsu Province, No. 1188 West No. two ring road Patentee after: Suzhou Shengze science and Technology Pioneer Park Development Co.,Ltd. Address before: 510663 Guangzhou high tech Industrial Development Zone, Guangdong Province, No. 3 spectrum East Road, A410 Patentee before: GUANGZHOU DAZHENG ADVANCED MATERIAL TECHNOLOGY Co.,Ltd. |
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