CN101497480A - Novel industrial water treatment agent and preparation thereof - Google Patents
Novel industrial water treatment agent and preparation thereof Download PDFInfo
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- CN101497480A CN101497480A CNA200910025405XA CN200910025405A CN101497480A CN 101497480 A CN101497480 A CN 101497480A CN A200910025405X A CNA200910025405X A CN A200910025405XA CN 200910025405 A CN200910025405 A CN 200910025405A CN 101497480 A CN101497480 A CN 101497480A
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- treatment agent
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 11
- 239000008235 industrial water Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- UANWURKQKKYIGV-UHFFFAOYSA-N 2-methoxypropan-1-amine Chemical compound COC(C)CN UANWURKQKKYIGV-UHFFFAOYSA-N 0.000 claims abstract description 15
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 8
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 7
- -1 2-methoxy propanamine dimethylene phosphonic acids Chemical class 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000005764 inhibitory process Effects 0.000 abstract description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 4
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract 3
- GXGJIOMUZAGVEH-UHFFFAOYSA-N Chamazulene Chemical group CCC1=CC=C(C)C2=CC=C(C)C2=C1 GXGJIOMUZAGVEH-UHFFFAOYSA-N 0.000 abstract 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 6
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229920000570 polyether Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000270666 Testudines Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 239000002455 scale inhibitor Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention relates to a novel industrial water treating agent 2-methoxy propylamine dimethylene phosphonic acid product and a method for preparing the same. The process for producing the product comprises that: firstly, 2-methoxy propylamine and water are added into a reaction kettle; when the temperature of the reaction kettle is controlled to be less than or equal to 50 DEG C, hydrochloric acid is dropwise added into the reaction kettle; phosphorous acid or phosphorus trichloride is added into the reaction kettle; after reaction is finished, formaldehyde is dropped to the mixture; the temperature is controlled to be between 85 and 105 DEG C; secondly, the temperature is controlled to be between 105 and 110 DEG C for reflux for 2 hours; acid water is distilled and reclaimed; the temperature is controlled to be between 1,108 and 125 DEG C; and finally, materials are cooled and reclaimed to obtain the product. Besides ether linkage, the product also contains phosphate groups and nitrogen; when the product is used in circulating water, the product has properties of scale inhibition and corrosion inhibition and has good using effect; and simultaneously, the product is also an environment-friendly type green water treatment agent.
Description
Technical field
The present invention relates to a kind of novel industrial water treatment agent and preparation method thereof, particularly 2-methoxy propanamine dimethylene phosphonic acids product and preparation method thereof.
Background technology
The recirculating cooling water system fouling is the problem that often runs in the industrial production; incrustation scale obviously descends the working efficiency of heat exchange system through regular meeting; the at present industrial method of adding phosphorous Scale inhibitors in the cooling water system that generally adopts prevents that the antipriming pipe wall corrodes and fouling.
Organic phospho acid is to use a widest class water conditioner at present, it is to many metal ions, have excellent huge legendary turtle as calcium, magnesium, iron and zinc etc. and close ability, scale inhibition ability to the inorganic salt crust, particularly carbonate of these metals is also very strong simultaneously, and in the domestic existing organic phosphine water conditioner, the overwhelming majority is only to contain a spot of functional group, for example only contain phosphate group, this limitation that just causes this class water conditioner to use is very big, and often is restricted in special field.
Having entered since the nineties in 20th century, is that the novel ether organic phospho acid that contains of representative is rapidly developed with polyamino polyether base methylenephosphonic acid, and polyether-based is introduced into organic phospho acid, makes its performance that breakthrough arranged.But, the product that contains ehter bond both at home and abroad in the organic phosphine water conditioner, general molecular weight is bigger than normal, itself just only plays throwing out in the water of high turbidity condition, if and the effective ingredient of medicament consumed, can influence scale inhibition effect, and, also not have good product to occur at present for the lower molecular weight organic phosphine water conditioner that contains ether.
Summary of the invention
Technical problem solved by the invention provides a kind of use and play scale effect in special recirculated water, strong anti-interference performance, novel industrial water treatment agent of better performances and environmental protection and preparation method thereof.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is to produce a kind of novel industrial water treatment agent, and the name of this water conditioner is called 2-methoxy propanamine dimethylene phosphonic acids, and has following structural formula:
Produce that the preparation method of above-mentioned industrial water conditioning agent undertakies by following processing step:
(1) be that the 2-methoxy propanamine of 4:1～6:1 and water drop in the reactor with mol ratio, the cooling dripping hydrochloric acid, add-on is 3～4 times of 2-methoxy propanamine mole number, control dropping temperature≤50 ℃;
(2) be that the phosphorous acid or the phosphorus trichloride of 2～3 times of 2-methoxy propanamines adds in the above-mentioned system with mole number, control dropping temperature≤55 ℃;
(3) heat to 85 ℃, drip formaldehyde, add-on is 10～12 times of 2-methoxy propanamine mole number, 85～105 ℃ of control dropping temperatures;
(4) insulation refluxed 2 hours, and temperature is controlled at 105～110 ℃;
(5) sour water, 110～125 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
For the further qualification of technical solution of the present invention, described phosphorous acid can be solid, also can be liquid.
The product of gained of the present invention is a low-molecular-weight organophosphorus product, and this product contains ehter bond, and from the molecular structure of product as can be seen, there are adelphotaxy in ehter bond and two phosphate groups, Ca in recirculated water
2+, Mg
2+Attraction force acts under, these metal ions can be by the firm complexing of this product, so this product has good scale inhibition performance in recirculated water; And because the existence of this product ehter bond, after mutual magnetism is cancelled out each other, degraded easily, reason is the mutual complexing Cheng Huanhou of O-Ca-P, and the bond energy of C-O-C reduces in the molecule, and chain rupture forms micromolecular compound easily, impels its decomposition; From the molecular structure of this product as can be seen, this product also contains phosphate group and nitrogen except that containing ehter bond in addition, therefore this product is used in recirculated water, has annexed scale inhibition characteristic and corrosion inhibition properties, has good result of use.
Simultaneously according to the dosage of this product in the recirculated water, in recirculated water this product working concentration at 3mg/L, and product content only 35%, therefore the total phosphorous in water only has 1.05mg/L (with PO
4Meter), adds and in water, plays the consumption of scale inhibition characteristic that therefore externally draining meets GB8978-1996 comprehensive discharge standard total phosphorus (with PO
4Meter)＜and the standard of 1.5mg/L, this product can be considered as the environment-friendly water conditioner.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Embodiment
The present invention is further detailed explanation below in conjunction with embodiment and accompanying drawing.
Embodiment 1
(1) drop into 225 kilograms of 2-methoxy propanamines and 225 kg of water in reactor, cooling drips 300 kilograms of hydrochloric acid, controlled temperature≤50 ℃;
(2) drip off and add 540 kilograms in phosphorous acid, control dropping temperature≤55 ℃;
(3) drip off and heat to 85 ℃, begin to drip 750 kilograms of formaldehyde, 85 ℃ of controlled temperature;
(4) drip off insulation and refluxed 2 hours, temperature is controlled at 105 ℃;
(5) sour water, 110 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
Embodiment 2
(1) drop into 225 kilograms of 2-methoxy propanamines and 180 kg of water in reactor, cooling drips 276 kilograms of hydrochloric acid, controlled temperature≤50 ℃;
(2) drip off and add 690 kilograms of phosphorus trichlorides, control dropping temperature≤55 ℃;
(3) drip off and heat to 85 ℃, begin to drip 830 kilograms of formaldehyde, 105 ℃ of controlled temperature;
(4) drip off insulation and refluxed 2 hours, temperature is controlled at 110 ℃;
(5) sour water, 120 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
Embodiment 3
(1) drop into 225 kilograms of 2-methoxy propanamines and 272 kg of water in reactor, cooling drips 368 kilograms of hydrochloric acid, controlled temperature≤50 ℃;
(2) drip off and add 1038 kilograms of phosphorus trichlorides, control dropping temperature≤55 ℃;
(3) drip off and heat to 85 ℃, begin to drip 908 kilograms of formaldehyde, 90 ℃ of controlled temperature;
(4) drip off insulation and refluxed 2 hours, temperature is controlled at 100 ℃;
(5) sour water, 120 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
Embodiment 4
(1) drop into 225 kilograms of 2-methoxy propanamines and 250 kg of water in reactor, cooling drips 300 kilograms of hydrochloric acid, controlled temperature≤50 ℃;
(2) drip off and add 620 kilograms of 80% phosphorous acid aqueous solutions, control dropping temperature≤55 ℃;
(3) drip off and heat to 85 ℃, begin to drip 860 kilograms of formaldehyde, 10 ℃ of controlled temperature;
(4) drip off insulation and refluxed 2 hours, temperature is controlled at 100 ℃;
(5) sour water, 110 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
Embodiment 5
(1) drop into 225 kilograms of 2-methoxy propanamines and 180 kg of water in reactor, cooling drips 280 kilograms of hydrochloric acid, controlled temperature≤50 ℃;
(2) drip off and add 415 kilograms in phosphorous acid, control dropping temperature≤55 ℃;
(3) drip off and heat to 85 ℃, begin to drip 750 kilograms of formaldehyde, 105 ℃ of controlled temperature;
(4) drip off insulation and refluxed 2 hours, temperature is controlled at 105 ℃;
(5) sour water, 110 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
Claims (3)
1, a kind of novel industrial water treatment agent is characterized in that the name of this water conditioner is called 2-methoxy propanamine dimethylene phosphonic acids, and has following structural formula:
2, a kind of preparation method of above-mentioned novel industrial water treatment agent is characterized in that this method undertaken by following processing step:
(1) be that the 2-methoxy propanamine of 4:1～6:1 and water drop in the reactor with mol ratio, the cooling dripping hydrochloric acid, add-on is 3～4 times of 2-methoxy propanamine mole number, control dropping temperature≤50 ℃;
(2) be that the phosphorous acid or the phosphorus trichloride of 2～3 times of 2-methoxy propanamines adds in the above-mentioned system with mole number, control dropping temperature≤55 ℃;
(3) heat to 85 ℃, drip formaldehyde, add-on is 10～12 times of 2-methoxy propanamine mole number, 85～105 ℃ of control dropping temperatures;
(4) insulation refluxed 2 hours, and temperature is controlled at 105～110 ℃;
(5) sour water, 110～125 ℃ of controlled temperature are reclaimed in distillation;
(6) cooling rewinding promptly obtains product.
3, the preparation method of novel industrial water treatment agent according to claim 2 is characterized in that: described phosphorous acid can be solid, also can be liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910025405XA CN101497480B (en) | 2009-03-02 | 2009-03-02 | Novel industrial water treatment agent and preparation thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910025405XA CN101497480B (en) | 2009-03-02 | 2009-03-02 | Novel industrial water treatment agent and preparation thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101497480A true CN101497480A (en) | 2009-08-05 |
| CN101497480B CN101497480B (en) | 2010-09-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910025405XA Expired - Fee Related CN101497480B (en) | 2009-03-02 | 2009-03-02 | Novel industrial water treatment agent and preparation thereof |
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| Country | Link |
|---|---|
| CN (1) | CN101497480B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072653A (en) * | 2014-07-14 | 2014-10-01 | 山东省泰和水处理有限公司 | Polypropylene methylenephosphonic acid and preparation method thereof |
| CN108358965A (en) * | 2018-02-27 | 2018-08-03 | 南通联膦化工有限公司 | A kind of preparation method of diglycolamine dimethylene-phosphonic acid |
-
2009
- 2009-03-02 CN CN200910025405XA patent/CN101497480B/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104072653A (en) * | 2014-07-14 | 2014-10-01 | 山东省泰和水处理有限公司 | Polypropylene methylenephosphonic acid and preparation method thereof |
| CN108358965A (en) * | 2018-02-27 | 2018-08-03 | 南通联膦化工有限公司 | A kind of preparation method of diglycolamine dimethylene-phosphonic acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101497480B (en) | 2010-09-29 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: JIANGHAI ENVIRONMENTAL PROTECTION CO., LTD. Free format text: FORMER NAME: JIANGSU JIANGHAI CHEMICAL INDUSTRY GROUP CO., LTD. |
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| CP01 | Change in the name or title of a patent holder |
Address after: Zheng Lu Jiao Town Wujin District 213116 Jiangsu city of Changzhou Province Patentee after: Jianghai Environmental Protection Co., Ltd. Address before: Zheng Lu Jiao Town Wujin District 213116 Jiangsu city of Changzhou Province Patentee before: Jiangsu Jianghai Chemical Group Co., Ltd. |
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| C56 | Change in the name or address of the patentee | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Zheng Lu Jiao Town Wujin District 213116 Jiangsu city of Changzhou Province Patentee after: JIANGHAI ENVIRONMENTAL PROTECTION CO., LTD. Address before: Zheng Lu Jiao Town Wujin District 213116 Jiangsu city of Changzhou Province Patentee before: Jianghai Environmental Protection Co., Ltd. |
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Effective date of registration: 20180124 Address after: 213127 Wei Village Industrial Park, spring river town, Xinbei District, Changzhou City, Jiangsu Patentee after: Changzhou Jiayou Chemical Co., Ltd. Address before: Zheng Lu Jiao Town Wujin District 213116 Jiangsu city of Changzhou Province Patentee before: JIANGHAI ENVIRONMENTAL PROTECTION CO., LTD. |
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Granted publication date: 20100929 Termination date: 20190302 |
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