CN103275120A - Low-trimethylene-content amino trimethylene phosphonic acid and preparation method thereof - Google Patents
Low-trimethylene-content amino trimethylene phosphonic acid and preparation method thereof Download PDFInfo
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- CN103275120A CN103275120A CN2013102188010A CN201310218801A CN103275120A CN 103275120 A CN103275120 A CN 103275120A CN 2013102188010 A CN2013102188010 A CN 2013102188010A CN 201310218801 A CN201310218801 A CN 201310218801A CN 103275120 A CN103275120 A CN 103275120A
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Abstract
The invention relates to a preparation method of low-trimethylene-content amino trimethylene phosphonic acid, which comprises the following specific processing steps: adding ammonium chloride, an amino trimethylene phosphonic acid mother solution and formalin into a reaction kettle, and increasing the temperature to 90 DEG C; dropwisely adding formaldehyde and phosphorous acid, and keeping refluxing while controlling the temperature; after the dropwise addition, performing refluxing reaction while keeping the temperature; detecting the phosphite content, supplementing formaldehyde, and further performing refluxing reaction while keeping the temperature; performing negative pressure outer evaporation to remove the ammonium chloride, the formaldehyde and hydrogen chloride; and cooling, and adding reverse osmosis water to regulate the active matter content. According to the invention, the provided amino trimethylene phosphonic acid has the characteristic of low trimethylene content (the active matter content is 50+/-2%, and the trimethylene content is 24-26%); and compared with the common commercially available amino trimethylene phosphonic acid, the provided amino trimethylene phosphonic acid has better compatibility with zinc corrosion inhibitor, and can regulate the amount of zinc corrosion inhibitor in a compound product in a wider range. Besides, the invention widens the application range of the amino trimethylene phosphonic acid in different water bodies.
Description
Technical field
The invention belongs to field of chemicals, a kind of low three methene Amino Trimethylene Phosphonic Acid and preparation method thereof are provided.
Background technology
Organic multicomponent phosphoric acid is external the mid-1960s exploitation, a class water conditioner that is identified the seventies.Have good chemical stability, high thermal resistance and have that consumption is few concurrently, advantage such as inhibition and scale effect.In addition, organic multicomponent phosphoric acid has excellent sequestering power to many metal ions, so be used for water treatment in a large number.The principal item of using has Amino Trimethylene Phosphonic Acid, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid and ethylene diamine tetra methylene phosphonic acid at present.Amino Trimethylene Phosphonic Acid is that cost is lower, one of kind that raw material is easy to get.
Amino Trimethylene Phosphonic Acid is the cathodic inhibiter, in water, can be dissociated into six positive ions and six negative ions, can form polynary ring inner complex with metal ions such as calcium, magnesium, and be scattered in the water with loose form, the normal crystallization of calcium dirt, magne-scale is damaged.Effect with good chelating, lower bound inhibition and lattice distortion, and has good chemical stability, facile hydrolysis not, ability comparatively high temps (200 ℃), and have inhibition and a scale-inhibiting properties, being used with other corrosion inhibiting and descaling agents, acting synergistically, is a kind of good alkaline water treatment agent.
The synthetic method of Amino Trimethylene Phosphonic Acid is more, is suitable for industrial synthetic method and mainly contains two kinds, and a kind of is the reaction of nitrilotriacetic acid and phosphorous acid, this method yield height, and good product quality, but raw material is difficult to obtain, and the cost height.Another kind method is to obtain through the single stage method reaction with ammonium salt (ammonium chloride, volatile salt etc.) with formaldehyde, phosphorous acid (or phosphorus trichloride).
Market sale now all is with these two kinds of technology products obtained therefrom Amino Trimethylene Phosphonic Acid in sum, and there is with the gluey muddiness of the composite easy appearance of zinc class inhibiter the not phenomenon of clear in the type product, prolongs in time to be agglomerated into precipitation gradually.Be unfavorable for use, storage and the transportation of composite product.
Summary of the invention
For solve existing commercially available Amino Trimethylene Phosphonic Acid with the composite product of zinc class inhibiter in the problem of turbidity and precipitation appears, bring into play the synergetic property of the excellence in its composite product, the invention provides a kind of low three methene Amino Trimethylene Phosphonic Acid and preparation method thereof, the composite product of this preparation method's products obtained therefrom is stable, the collaborative effect | fruit is good, satisfies the more demand of the composite adjusting of wide region.
In order to achieve the above object, the invention provides a kind of low three methene Amino Trimethylene Phosphonic Acid and its preparation method is provided.The preparation technology who takes is for dripping formaldehyde and phosphorous acid reacting by heating in ATMP mother liquor, ammonium chloride and the formalin mixed solution, boils off outward except hydrogenchloride and responseless ammonium chloride, formaldehyde, adds reverse osmosis water and regulates active matter content.
A kind of low three methene Amino Trimethylene Phosphonic Acid preparation methods, concrete processing step is:
(1) ammonium chloride, Amino Trimethylene Phosphonic Acid mother liquor and formalin are added reactor, improve temperature to 90 ℃;
(2) drip formaldehyde and phosphorous acid, the control temperature keeps refluxing;
(3) dropwise the backflow insulation reaction;
(4) detect inferior phosphorus content and add formaldehyde, continue the insulation back flow reaction;
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrogenchloride;
(6) cooling adds reverse osmosis water and regulates active matter content.
The low three methene Amino Trimethylene Phosphonic Acid of above-mentioned explained hereafter, it is characterized in that: three methene content are 24 ~ 26%, active matter content is 50 ± 2%.
The mol ratio of such scheme step (1) and (2) described ammonium chloride, formaldehyde and phosphorous acid is 1:1.5 ~ 3:1.5 ~ 3, preferably 1:2 ~ 3:1.5 ~ 2.5.
The described Amino Trimethylene Phosphonic Acid mother liquor of above-mentioned steps (1) is for producing the mother liquor of crystal Amino Trimethylene Phosphonic Acid, and add-on is 15 ~ 60% of phosphorous acid, formaldehyde and ammonium chloride total mass, and preferably 20 ~ 35%.
Above-mentioned (1) described formalin is the organic phosphine by product, and wherein formaldehyde content is the formaldehyde waste water solution of 5 ~ 30ppm.
The addition of above-mentioned (1) and (2) described formalin is 0 ~ 30% of phosphorous acid, formaldehyde and ammonium chloride total mass.
The dropping of above-mentioned (2) described phosphorous acid and formaldehyde, formaldehyde should be postponed 10 ~ 30min than phosphorous acid and be dropwised.
The temperature that insulation refluxes in above-mentioned (3) is 105 ~ 120 ℃.
The time of insulation back flow reaction is 1 ~ 4h in above-mentioned (3).
The additional amount of formaldehyde in above-mentioned (4) is as phosphorous acid content (PO
3 3-)≤3.5% an o'clock formaldehyde additional amount is 0, as phosphorous acid content (PO
3 3-)＞3.5% o'clock, formaldehyde additional amount and remaining phosphorous acid mol ratio are 1.0 ~ 1.5:1.
The amount as if adding formaldehyde described in above-mentioned (4) is not 0, and the time of continuing insulation reaction is 1h.
Hydrogenchloride absorbs with the falling film absorption device and makes 30% hydrochloric acid in above-mentioned (5), and ammonium chloride and formaldehyde are as the raw material recycling.
Excellent benefit of the present invention is: the Amino Trimethylene Phosphonic Acid that provides has the characteristics of three methene content low (active matter content 50 ± 2%, three methene content are 24 ~ 26%).To compare zinc class inhibiter compatibility performance good with common commercially available Amino Trimethylene Phosphonic Acid, can regulate the amount of zinc class inhibiter in the composite product at wide region more.Enlarged the use range of Amino Trimethylene Phosphonic Acid in different quality.
This invention preparation technology rationally utilized production crystal Amino Trimethylene Phosphonic Acid residue mother liquor, solved the extra-expense of production liquid waste disposal discharging and to the harm problem of environment.
Specific embodiment
Embodiment 1
A kind of low three methene Amino Trimethylene Phosphonic Acid specifically prepare implementing process and are:
(1) 500kg ammonium chloride, 480kgATMP mother liquor are joined reactor, add 500kg formalin simultaneously, improve temperature to 90 ℃.
(2) drip 1580kg phosphorous acid and 1640kg formaldehyde simultaneously, the control temperature keeps refluxing, and formaldehyde is postponed 15min than phosphorous acid and dropwised.
(3) formaldehyde dropwises 110 ± 2 ℃ of back flow reaction 2h of control temperature.
(4) detect phosphorous acid content, add formaldehyde 100kg, continue insulation backflow 1h.
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrochloric acid.
(6) near normal temperature adds the 3200kg reverse osmosis water and regulates active matter content 50 ± 2%.
Embodiment 2
A kind of low three methene Amino Trimethylene Phosphonic Acid specifically prepare implementing process and are:
(1) 500kg ammonium chloride, 450kgATMP mother liquor are joined reactor, add 700kg formalin simultaneously, improve temperature to 90 ℃.
(2) drip 1550kg phosphorous acid and 1680kg formaldehyde simultaneously, the control temperature keeps refluxing, and formaldehyde is postponed 20min than phosphorous acid and dropwised.
(3) formaldehyde dropwises 105 ± 2 ℃ of back flow reaction 3h of control temperature.
(4) detect phosphorous acid content, add formaldehyde 75kg, continue insulation backflow 1h.
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrochloric acid.
(6) near normal temperature adds the 4000kg reverse osmosis water and regulates active matter content 50 ± 2%.
Embodiment 3
A kind of low three methene Amino Trimethylene Phosphonic Acid specifically prepare implementing process and are:
(1) 550kg ammonium chloride, 450kgATMP mother liquor are joined reactor, add 700kg formalin simultaneously, improve temperature to 90 ℃.
(2) drip 1550kg phosphorous acid and 1700kg formaldehyde simultaneously, the control temperature keeps refluxing, and formaldehyde is postponed 20min than phosphorous acid and dropwised.
(3) formaldehyde dropwises 105 ± 2 ℃ of back flow reaction 3h of control temperature.
(4) detect phosphorous acid content.
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrochloric acid.
(6) near normal temperature adds the 3850kg reverse osmosis water and regulates active matter content 50 ± 2%.
Embodiment 4
A kind of low three methene Amino Trimethylene Phosphonic Acid specifically prepare implementing process and are:
(1) 500kg ammonium chloride, 600kgATMP mother liquor are joined reactor, add 300kg formalin simultaneously, improve temperature to 90 ℃.
(2) drip 1550kg phosphorous acid and 1680kg formaldehyde simultaneously, the control temperature keeps refluxing, and formaldehyde is postponed 20min than phosphorous acid and dropwised.
(3) formaldehyde dropwises 115 ± 2 ℃ of back flow reaction 3h of control temperature.
(4) detect phosphorous acid content, add formaldehyde 83kg, continue insulation backflow 1h.
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrochloric acid.
(6) near normal temperature adds the 4000kg reverse osmosis water and regulates active matter content 50 ± 2%.
Embodiment 5
A kind of low three methene Amino Trimethylene Phosphonic Acid specifically prepare implementing process and are:
(1) 500kg ammonium chloride, 600kgATMP mother liquor are joined reactor, improve temperature to 90 ℃.
(2) drip 1550kg phosphorous acid and 1680kg formaldehyde simultaneously, the control temperature keeps refluxing, and formaldehyde is postponed 20min than phosphorous acid and dropwised.
(3) formaldehyde dropwises 115 ± 2 ℃ of back flow reaction 3h of control temperature.
(4) detect phosphorous acid content, add formaldehyde 75kg, continue insulation backflow 1h.
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrochloric acid.
Near normal temperature adds the 3960kg reverse osmosis water and regulates active matter content 50 ± 2%.
Claims (10)
1. one kind is hanged down three methene Amino Trimethylene Phosphonic Acid preparation methods, and processing step is:
(1) ammonium chloride, Amino Trimethylene Phosphonic Acid mother liquor and formalin are added reactor, improve temperature to 90 ℃;
(2) drip formaldehyde and phosphorous acid, the control temperature keeps refluxing;
(3) dropwise the backflow insulation reaction;
(4) detect inferior phosphorus content and add formaldehyde, continue the insulation back flow reaction;
(5) the outer steaming of negative pressure removed ammonium chloride, formaldehyde and hydrogenchloride;
(6) cooling adds reverse osmosis water and regulates active matter content.
2. the low three methene Amino Trimethylene Phosphonic Acid of the described explained hereafter of claim 1, it is characterized in that: three methene content are 24 ~ 26%, active matter content is 50 ± 2%.
3. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 1, it is characterized in that: the mol ratio of step in the such scheme (1) and (2) described ammonium chloride, formaldehyde and phosphorous acid is 1:1.5 ~ 3:1.5 ~ 3.
4. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 3, it is characterized in that: the mol ratio of step in the such scheme (1) and (2) described ammonium chloride, formaldehyde and phosphorous acid is 1:2 ~ 3:1.5 ~ 2.5.
5. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 3, it is characterized in that: the Amino Trimethylene Phosphonic Acid mother liquor described in the above-mentioned steps (1) is for producing the mother liquor of crystal Amino Trimethylene Phosphonic Acid, and add-on is 15 ~ 60% of phosphorous acid, formaldehyde and ammonium chloride total mass.
6. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 5, it is characterized in that: the Amino Trimethylene Phosphonic Acid mother liquor described in the above-mentioned steps (1) is for producing the mother liquor of crystal Amino Trimethylene Phosphonic Acid, and add-on is 20 ~ 35% of phosphorous acid, formaldehyde and ammonium chloride total mass; The described formalin of above-mentioned steps (1) is the organic phosphine by product, and wherein formaldehyde content is the formaldehyde waste water solution of 5 ~ 30ppm.
7. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 1, it is characterized in that: the addition of above-mentioned steps (1) and (2) described formalin is 0 ~ 30% of phosphorous acid, formaldehyde and ammonium chloride total mass.
8. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 3, it is characterized in that: the dropping of the described phosphorous acid of above-mentioned steps (2) and formaldehyde, formaldehyde should be postponed 10 ~ 30min than phosphorous acid and be dropwised.
9. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 1, it is characterized in that: the temperature that insulation refluxes in the above-mentioned steps (3) is 105 ~ 120 ℃; The time of insulation back flow reaction is 1 ~ 4h.
10. the preparation method of a kind of low three methene Amino Trimethylene Phosphonic Acid according to claim 3 is characterized in that: the additional amount of formaldehyde in the above-mentioned steps (4), and as phosphorous acid content (PO
3 3-)≤3.5% an o'clock formaldehyde additional amount is 0, as phosphorous acid content (PO
3 3-)＞3.5% o'clock, formaldehyde additional amount and remaining phosphorous acid mol ratio are 1.0 ~ 1.5:1; If adding the amount of formaldehyde is not 0, the time of continuing insulation reaction is 1h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694274A (en) * | 2014-01-16 | 2014-04-02 | 山东省泰和水处理有限公司 | Preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid |
| CN103708637A (en) * | 2014-01-02 | 2014-04-09 | 山东省泰和水处理有限公司 | Amino trimethylene phosphonic acid-N-oxide and preparation method thereof |
| CN106518919A (en) * | 2016-08-31 | 2017-03-22 | 南通联膦化工有限公司 | Technology used for producing amino trimethylene phosphoric acid and salts thereof and capable of reusing formaldehyde wastewater |
| CN107573377A (en) * | 2017-09-09 | 2018-01-12 | 南通意特化工有限公司 | Can the aminotrimethylene phosphoric acid of reuse formaldehyde waste water and its production technology of salt |
| CN107722361A (en) * | 2017-09-26 | 2018-02-23 | 同济大学 | A kind of preparation method of the magnesium-supported redox graphene fire retardant of nanometer of ATMP |
| CN108276441A (en) * | 2018-01-31 | 2018-07-13 | 山东大学 | The preparation method of two methylenephosphonic acid of cyclohexylamine |
| CN110804071A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
| CN110804070A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of amino trimethylene phosphonic acid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103708637A (en) * | 2014-01-02 | 2014-04-09 | 山东省泰和水处理有限公司 | Amino trimethylene phosphonic acid-N-oxide and preparation method thereof |
| CN103694274A (en) * | 2014-01-16 | 2014-04-02 | 山东省泰和水处理有限公司 | Preparation method of low-chloride low-ammonia amino trimethylene phosphonic acid |
| CN106518919A (en) * | 2016-08-31 | 2017-03-22 | 南通联膦化工有限公司 | Technology used for producing amino trimethylene phosphoric acid and salts thereof and capable of reusing formaldehyde wastewater |
| CN107573377A (en) * | 2017-09-09 | 2018-01-12 | 南通意特化工有限公司 | Can the aminotrimethylene phosphoric acid of reuse formaldehyde waste water and its production technology of salt |
| CN107722361A (en) * | 2017-09-26 | 2018-02-23 | 同济大学 | A kind of preparation method of the magnesium-supported redox graphene fire retardant of nanometer of ATMP |
| CN108276441A (en) * | 2018-01-31 | 2018-07-13 | 山东大学 | The preparation method of two methylenephosphonic acid of cyclohexylamine |
| CN110804071A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
| CN110804070A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of amino trimethylene phosphonic acid |
| WO2021088457A1 (en) * | 2019-11-08 | 2021-05-14 | 山东泰和水处理科技股份有限公司 | Method for producing diethylenetriaminepenta(methylene-phosphonic acid) |
| WO2021088449A1 (en) * | 2019-11-08 | 2021-05-14 | 山东泰和水处理科技股份有限公司 | Method for producing amino trimethylene phosphonic acid |
| CN110804070B (en) * | 2019-11-08 | 2021-09-17 | 山东泰和水处理科技股份有限公司 | Production method of amino trimethylene phosphonic acid |
| CN110804071B (en) * | 2019-11-08 | 2021-09-17 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
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Address after: Shandong Hong Village 277000 Zaozhuang City District Xi Wang Zhuang Xiang Applicant after: SHANDONG TAIHE WATER TREATMENT TECHNOLOGIES CO., LTD. Address before: Shandong Hong Village 277000 Zaozhuang City District Xi Wang Zhuang Xiang Applicant before: Shandong Taihe Water Treatment Co., Ltd. |
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Application publication date: 20130904 |