CN103420510A - Preparation method of tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor - Google Patents
Preparation method of tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor Download PDFInfo
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- CN103420510A CN103420510A CN2012101640379A CN201210164037A CN103420510A CN 103420510 A CN103420510 A CN 103420510A CN 2012101640379 A CN2012101640379 A CN 2012101640379A CN 201210164037 A CN201210164037 A CN 201210164037A CN 103420510 A CN103420510 A CN 103420510A
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- phosphonic acid
- trimethylene phosphonic
- amino trimethylene
- sodium
- sodium salt
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Abstract
The invention discloses a preparation method of a tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor, belonging to the field of chemical engineering. Raw materials of tetra sodium salt of amino trimethylene phosphonic acid, polyol phosphonate, hydroxyethanediphosphonic acid potassium salt and sodium polyepoxysuccinic acid react in a reaction kettle container for a certain time at proper temperature to prepare the tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor. The method has advantages of simple production technology, low cost and no discharge of ''three wastes''; and besides excellent scale inhibition effect, the tetra sodium salt of amino trimethylene phosphonic acid has excellent corrosion inhibition effect, especially has excellent scale inhibition effect and excellent corrosion inhibition effect on an enclosed recirculated cooling water system.
Description
Technical field
Product of the present invention belongs to chemical field, relates in particular to a kind of compound method of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss.
Background technology
Amino Trimethylene Phosphonic Acid four sodium claim again Amino Trimethylene Phosphonic Acid four sodium, and molecular formula is C3H8NO9P3Na4, and outward appearance is colourless or light yellow transparent liquid, and relative molecular mass is 387.Amino Trimethylene Phosphonic Acid four sodium are neutral sodium-salts of Amino Trimethylene Phosphonic Acid, as Scale inhibitors, use, can stop scaling salt class in water to form incrustation scale, the particularly formation of calcium carbonate scale, Amino Trimethylene Phosphonic Acid four sodium can being used as Scale inhibitors in the recirculated cooling water of fuel-burning power plant, refinery, oil field reinjection water system.The Scale inhibitors of Amino Trimethylene Phosphonic Acid four sodium and other has good consistency, can be re-dubbed water conditioner with organic phospho acid, poly carboxylic acid or polycarboxylate etc., to be adapted to the recirculating cooling water system of different quality condition, and without the ammonia flavor, produces while using.It is main raw material that Amino Trimethylene Phosphonic Acid four sodium are take in the present invention, take polyvalent alcohol phosphonates, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium, polyepoxy sodium succinate is auxiliary material, take chemical reaction kettle as container, being aided with suitable temperature and reaction times prepares ethylene diamine tetra methylene phosphonic acid sodium composite Scale inhibitors, there is production technique simple, with low cost, without the advantage of " three wastes " discharge.Wherein the effect of polyvalent alcohol phosphonates is: owing to having introduced a plurality of polyoxyethylene groups in molecule, can greatly improve corrosion inhibition, barium in water, strontium dirt deposition are had to good restraining effect, the difficulty soluble salts such as the calcium carbonate in water, calcium sulfate deposition is also had to good scale effect, steel are had to the galvanic protection effect; 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium is sylvite, compares with sodium salt and have higher solubleness under neutrallty condition, is the inhibitor of excellent calcium carbonate scale; Polyepoxy sodium succinate is the polynary anti-incrustation corrosion inhibitor of a kind of environment-friendly type, calcium carbonate in water, calcium sulfate, barium sulfate, Calcium Fluoride (Fluorspan) and silicon dirt are had to good scale inhibition and dispersion performance, there is good synergistic function with phosphonate is composite, be particularly useful for the cooling water system under high-alkali, high hard, high PH condition.Amino Trimethylene Phosphonic Acid four sodium, except fabulous scale effect is arranged, also have good corrosion mitigating effect, especially good to closed circulation cooling water system scale inhibition, corrosion mitigating effect.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of method that batch prepares Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss, this product is with Amino Trimethylene Phosphonic Acid four sodium, the polyvalent alcohol phosphonates, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium, polyepoxy sodium succinate is raw material, take chemical reaction kettle as container, be aided with suitable temperature and reaction times, prepare Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss, the proportioning raw materials of producing this product use is: Amino Trimethylene Phosphonic Acid four sodium 70%-72%, polyvalent alcohol phosphonates 10%-12%, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium 10%, polyepoxy sodium succinate 8%.
The present invention can be achieved through the following technical solutions:
A kind of compound method of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss, its feature consists of following steps:
(1) Amino Trimethylene Phosphonic Acid of formula ratio four sodium, polyvalent alcohol phosphonates being started to stirrer after sending in chemical reaction kettle stirs, rotating speed is 25 rev/mins, send into steam immediately in the reactor interlayer, make slowly to heat up in reactor, control temperature between 40 ℃-45 ℃, stirring reaction 1 hour.
(2) stop the steam supply to reactor, be cooled between 25 ℃-30 ℃, continue to stir, add 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium, the polyepoxy sodium succinate of formula ratio simultaneously, stir after 0.5 hour and stop stirring, obtain finished product after being cooled to normal temperature.
Temperature in above-mentioned steps (1) is 43 ℃.
Temperature in above-mentioned steps (2) is 28 ℃.
The invention has the beneficial effects as follows: the production method that a kind of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss are provided; this production method has the advantages such as technique is simple, reaction conditions is gentle, production cost is low, good product quality; product has good restraining effect to the barium in water, strontium dirt deposition; the difficulty soluble salts such as the calcium carbonate in water, calcium sulfate deposition is also had to good scale effect, steel are had to the galvanic protection effect.
Embodiment
Embodiment 1
By accounting for Amino Trimethylene Phosphonic Acid four sodium that total amount is 70%, account for after polyvalent alcohol phosphonates that total amount is 12% is sent in chemical reaction kettle and start stirrer and stir, rotating speed is 25 rev/mins, send into steam immediately in the reactor interlayer, make slowly to heat up in reactor, control temperature between 40 ℃-45 ℃, stirring reaction 1 hour; Stop the steam supply to reactor, be cooled between 25 ℃-30 ℃, continue to stir, add to account for 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium that total amount is 10%, account for the polyepoxy sodium succinate that total amount is 8% simultaneously, stir after 0.5 hour and stop stirring, obtain finished product after being cooled to normal temperature.
Embodiment 2
By accounting for Amino Trimethylene Phosphonic Acid four sodium that total amount is 71%, account for after polyvalent alcohol phosphonates that total amount is 11% is sent in chemical reaction kettle and start stirrer and stir, rotating speed is 25 rev/mins, send into steam immediately in the reactor interlayer, make slowly to heat up in reactor, control temperature between 40 ℃-45 ℃, stirring reaction 1 hour; Stop the steam supply to reactor, be cooled between 25 ℃-30 ℃, continue to stir, add to account for 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium that total amount is 10%, account for the polyepoxy sodium succinate that total amount is 8% simultaneously, stir after 0.5 hour and stop stirring, obtain finished product after being cooled to normal temperature.
Embodiment 3
By accounting for Amino Trimethylene Phosphonic Acid four sodium that total amount is 72%, account for after polyvalent alcohol phosphonates that total amount is 10% is sent in chemical reaction kettle and start stirrer and stir, rotating speed is 25 rev/mins, send into steam immediately in the reactor interlayer, make slowly to heat up in reactor, control temperature between 40 ℃-45 ℃, stirring reaction 1 hour; Stop the steam supply to reactor, be cooled between 25 ℃-30 ℃, continue to stir, add to account for 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium that total amount is 10%, account for the polyepoxy sodium succinate that total amount is 8% simultaneously, stir after 0.5 hour and stop stirring, obtain finished product after being cooled to normal temperature.
Claims (3)
1. the compound method of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss, its composition of raw materials counts by weight percentage, and comprising: Amino Trimethylene Phosphonic Acid four sodium 70%-72%, polyvalent alcohol phosphonates 10%-12%, 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium 10%, polyepoxy sodium succinate 8%; It is characterized in that: step (1) is started stirrer and is stirred after sending the Amino Trimethylene Phosphonic Acid of formula ratio four sodium, polyvalent alcohol phosphonates in chemical reaction kettle, rotating speed is 25 rev/mins, send into steam immediately in the reactor interlayer, make slowly to heat up in reactor, control temperature between 40 ℃-45 ℃, stirring reaction 1 hour; Step (2) stops the steam supply to reactor, is cooled between 25 ℃-30 ℃, continue to stir, and adds 1-Hydroxy Ethylidene-1,1-Diphosphonic Acid potassium, the polyepoxy sodium succinate of formula ratio simultaneously, stirs after 0.5 hour and stops stirring, and obtains finished product after being cooled to normal temperature.
2. the compound method of a kind of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss according to claim 1, the feature of its step (1) is: described temperature is 43 ℃.
3. the compound method of a kind of Amino Trimethylene Phosphonic Acid four sodium composite Scale inhibitorss according to claim 1, the feature of its step (2) is: described temperature is 28 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101640379A CN103420510A (en) | 2012-05-25 | 2012-05-25 | Preparation method of tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor |
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| CN2012101640379A CN103420510A (en) | 2012-05-25 | 2012-05-25 | Preparation method of tetra sodium salt of amino trimethylene phosphonic acid compound scale inhibitor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755147A (en) * | 2014-01-14 | 2014-04-30 | 清华大学 | Etching liquid and preparation method and application thereof |
| CN104891685A (en) * | 2015-05-19 | 2015-09-09 | 山东省泰和水处理有限公司 | A synthesis process of 1,3-cyclohexanebis(methylamine) tetra(methylenephosphonic acid) |
| RU2580685C2 (en) * | 2014-07-04 | 2016-04-10 | Акционерное общество "Химический завод им. Л.Я. Карпова" | Corrosion and scaling inhibitor |
| CN106479467A (en) * | 2016-08-30 | 2017-03-08 | 陕西省石油化工研究设计院 | A kind of environment-friendly type is fluorinated calcium inhibitorses |
-
2012
- 2012-05-25 CN CN2012101640379A patent/CN103420510A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755147A (en) * | 2014-01-14 | 2014-04-30 | 清华大学 | Etching liquid and preparation method and application thereof |
| CN103755147B (en) * | 2014-01-14 | 2016-03-30 | 清华大学 | Etching solution and preparation method thereof and application |
| RU2580685C2 (en) * | 2014-07-04 | 2016-04-10 | Акционерное общество "Химический завод им. Л.Я. Карпова" | Corrosion and scaling inhibitor |
| CN104891685A (en) * | 2015-05-19 | 2015-09-09 | 山东省泰和水处理有限公司 | A synthesis process of 1,3-cyclohexanebis(methylamine) tetra(methylenephosphonic acid) |
| CN106479467A (en) * | 2016-08-30 | 2017-03-08 | 陕西省石油化工研究设计院 | A kind of environment-friendly type is fluorinated calcium inhibitorses |
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Application publication date: 20131204 |