CN105439295A - Preparation method for degradable slow-release scale inhibitor - Google Patents

Abstract

The invention relates to a preparation method for a degradable slow-release scale inhibitor, and belongs to the technical field of scale inhibitor preparation. The preparation method comprises the steps that maleic acid is added into deionized water, after heating in a water bath and cooling are performed, an aqueous ammonia solution is added, heating is performed to increase the temperature, and stirring, drying and cyclodehydration are performed to obtain a yellow solid; the yellow solid is added into distilled water, heating is performed to increase the temperature, and titration and hydrolysis are performed with a sodium hydroxide solution; after the color of the solution is changed into reddish brown, heating is stopped, and natural cooling and standing are performed; filtering is performed, collected filtrate is added into absolute methanol, and precipitation is performed; filtering is performed, filtrate is collected, evaporated and dried, and a granular scale inhibitor is prepared; the granular scale inhibitor is mixed with substances such as a gelatin solution, standing and defoaming are performed, drying is performed, and then the scale inhibitor is prepared. The preparation method has the advantages that when the prepared degradable slow-release scale inhibitor is put into an environment needing scale inhibition, the scale inhibitor is easy to decompose, friendly to the environment and good in scale inhibiting effect, cannot cause water eutrophication and does not need to be massively put due to the slow-release effect of the scale inhibitor.

Description

A kind of preparation method of degradable controlled release Scale inhibitors

Technical field

The present invention relates to a kind of preparation method of degradable controlled release Scale inhibitors, belong to Scale inhibitors preparing technical field.

Background technology

Scale inhibitors (scaleinhibitor): be the insoluble inorganic salt had in energy disperse water, prevention or the precipitation of interference insoluble inorganic salt in metallic surface, fouling function, and maintain the class medicament that hardware has good heat-transfer effect.Cold exchange device antiseptic corrosion inhibitor is with epoxy resin and specific amino resin for base-material, and it is formulated to add the appropriate various auxiliary agent such as various antirust, anticorrosion, is single component.It has excellent shielding, impervious, rustless property, good scale inhibition, thermal conductivity, the performances such as excellent weak acid resistant, highly basic, organic solvent, its strong adhesion, and rete is bright, pliable and tough, fine and close, hard.

At present for swimming pool, particularly the scale problems of Spa and hot tube adds the Scale inhibitors of high dosage (40-50ppm) to reach the object of scale inhibition with usually adopting regular intervals of time (every 2-4 week).The most frequently used Scale inhibitors is ortho-phosphoric an alkali metal salt.But this dosing method may cause Scale inhibitors too high levels in early stage, and Scale inhibitors approach exhaustion before once feeding intake on the later stage may occur in, cause the phenomenon that fouling occurs.In addition, because the solubleness of calcium phosphate is very little, when phosphorus acid ion concentration is excessive, not only can not play scale inhibition effect, make fouling more serious on the contrary, and the more difficult removing of fouling that the fouling of calcium phosphate formation causes more than calcium carbonate and Calcium hydrogen carbonate.

Summary of the invention

The technical problem that the present invention mainly solves: be Scale inhibitors for ortho-phosphoric an alkali metal salt, not only need to add in a large number, and after being used to complete, meeting fouling, the problem of scale inhibition effect difference, provide in a kind of particle Scale inhibitors preparing and add the materials such as gelatin, mix, standing and defoaming obtains the method for degradable controlled release Scale inhibitors, and degradable controlled release Scale inhibitors prepared by the present invention is fed in required scale inhibition environment, easy decomposition, can not cause body eutrophication, environmentally friendly, scale inhibition effect is good, due to the effect of its slowly-releasing, without the need to adding in a large number.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:

(1) 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 70 ~ 80 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 10 ~ 15min, stop subsequently heating and making it naturally cool to 20 ~ 25 DEG C, be prepared into maleic acid solution;

(2) 1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 80 ~ 90 DEG C subsequently, make its stirring reaction 3 ~ 5h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 1 ~ 2h at 160 ~ 180 DEG C, cyclodehydration 3 ~ 4h in 210 ~ 230 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently;

(3) 1:10 in mass ratio, the yellow solid of above-mentioned preparation is added in distilled water, after being heated to 50 ~ 60 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 1 ~ 2h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 1 ~ 2h, it filtered and collects filtrate;

(4) 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under rotating speed 600 ~ 800r/min, make its Precipitation, after 45 ~ 60min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 50 ~ 60 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use;

(5) 1:5 in mass ratio, gelatin is dissolved in distilled water at 55 ~ 60 DEG C, be uniformly mixed 10 ~ 15min and be prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 30 ~ 45 parts, 10 ~ 15 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 45 ~ 55 parts, 30 ~ 45min is uniformly mixed at 600 ~ 800r/min, subsequently after standing and defoaming 2 ~ 3h, be placed in stainless steel mould, under 2 ~ 3MPa, lucifuge drying 4 ~ 5 days, can be prepared into degradable controlled release Scale inhibitors.

Application of the present invention: after 1:120 ~ 1:100 mixes in mass ratio by degradable controlled release Scale inhibitors and the water of above-mentioned preparation, behind the wall being evenly sprayed at swimming pool and bottom, the degradable controlled release Scale inhibitors of above-mentioned preparation is added again in swimming pool, the amount added in water per ton is 2 ~ 3g, from bottom, air is filled with to it, aeration 10 ~ 15min, uses this degradable controlled release Scale inhibitors, wall and bottom do not have fouling, and water body keeps clean simultaneously.

The invention has the beneficial effects as follows:

(1) be fed in required scale inhibition environment, easily decompose, can not body eutrophication be caused, environmentally friendly;

(2) scale inhibition effect is good, due to the effect of its slowly-releasing, without the need to adding in a large number;

(3) preparation process is simple, and cost is low.

Embodiment

First 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 70 ~ 80 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 10 ~ 15min, stop subsequently heating and making it naturally cool to 20 ~ 25 DEG C, be prepared into maleic acid solution;

1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 80 ~ 90 DEG C subsequently, make its stirring reaction 3 ~ 5h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 1 ~ 2h at 160 ~ 180 DEG C, cyclodehydration 3 ~ 4h in 210 ~ 230 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently; 1:10 in mass ratio again, the yellow solid of above-mentioned preparation is added in distilled water, after being heated to 50 ~ 60 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 1 ~ 2h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 1 ~ 2h, it filtered and collects filtrate; 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under 600 ~ 800r/min, make its Precipitation, after 45 ~ 60min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 50 ~ 60 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use; 1:5 in mass ratio, gelatin is dissolved in distilled water at 55 ~ 60 DEG C, be uniformly mixed 10 ~ 15min and be prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 30 ~ 45 parts, 10 ~ 15 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 45 ~ 55 parts, 30 ~ 45min is uniformly mixed at 600 ~ 800r/min, subsequently after standing and defoaming 2 ~ 3h, be placed in stainless steel mould, under 2 ~ 3MPa, lucifuge drying 4 ~ 5 days, can be prepared into degradable controlled release Scale inhibitors.

Example 1

First 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 80 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 15min, stop subsequently heating and making it naturally cool to 25 DEG C, be prepared into maleic acid solution; 1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 90 DEG C subsequently, make its stirring reaction 5h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 2h at 180 DEG C, cyclodehydration 4h in 230 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently; 1:10 in mass ratio again, is added in distilled water by the yellow solid of above-mentioned preparation, after being heated to 60 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 2h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 2h, it filtered and collects filtrate; 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under 800r/min, make its Precipitation, after 60min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 60 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use; 1:5 in mass ratio, gelatin is dissolved in distilled water at 60 DEG C, is uniformly mixed 15min and is prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 45 parts, 10 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 45 parts, is uniformly mixed 45min at 600r/min, subsequently after standing and defoaming 3h, be placed in stainless steel mould, under 3MPa, dry 5 days of lucifuge, can be prepared into degradable controlled release Scale inhibitors.After by the degradable controlled release Scale inhibitors of above-mentioned preparation, 1:120 mixes in mass ratio with water, behind the wall being evenly sprayed at swimming pool and bottom, the degradable controlled release Scale inhibitors of above-mentioned preparation is added again in swimming pool, the amount added in water per ton is 3g, from bottom, air is filled with to it, aeration 15min, uses this degradable controlled release Scale inhibitors, wall and bottom do not have fouling, and water body keeps clean simultaneously.

Example 2

First 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 70 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 10min, stop subsequently heating and making it naturally cool to 20 DEG C, be prepared into maleic acid solution; 1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 80 DEG C subsequently, make its stirring reaction 3h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 1h at 160 DEG C, cyclodehydration 3h in 210 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently; 1:10 in mass ratio again, is added in distilled water by the yellow solid of above-mentioned preparation, after being heated to 50 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 1h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 1h, it filtered and collects filtrate; 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under 600r/min, make its Precipitation, after 45min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 50 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use; 1:5 in mass ratio, gelatin is dissolved in distilled water at 55 DEG C, is uniformly mixed 10min and is prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 30 parts, 15 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 55 parts, is uniformly mixed 30min at 600r/min, subsequently after standing and defoaming 2h, be placed in stainless steel mould, under 2MPa, dry 4 days of lucifuge, can be prepared into degradable controlled release Scale inhibitors.After by the degradable controlled release Scale inhibitors of above-mentioned preparation, 1:100 mixes in mass ratio with water, behind the wall being evenly sprayed at swimming pool and bottom, the degradable controlled release Scale inhibitors of above-mentioned preparation is added again in swimming pool, the amount added in water per ton is 2g, from bottom, air is filled with to it, aeration 10min, uses this degradable controlled release Scale inhibitors, wall and bottom do not have fouling, and water body keeps clean simultaneously.

Example 3

First 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 75 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 12min, stop subsequently heating and making it naturally cool to 22 DEG C, be prepared into maleic acid solution; 1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 85 DEG C subsequently, make its stirring reaction 4h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 1h at 170 DEG C, cyclodehydration 3h in 220 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently; 1:10 in mass ratio again, is added in distilled water by the yellow solid of above-mentioned preparation, after being heated to 55 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 1h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 1h, it filtered and collects filtrate; 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under 700r/min, make its Precipitation, after 50min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 55 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use; 1:5 in mass ratio, gelatin is dissolved in distilled water at 57 DEG C, is uniformly mixed 12min and is prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 40 parts, 15 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 45 parts, is uniformly mixed 40min at 700r/min, subsequently after standing and defoaming 2h, be placed in stainless steel mould, under 2MPa, dry 4 days of lucifuge, can be prepared into degradable controlled release Scale inhibitors.After by the degradable controlled release Scale inhibitors of above-mentioned preparation, 1:100 mixes in mass ratio with water, behind the wall being evenly sprayed at swimming pool and bottom, the degradable controlled release Scale inhibitors of above-mentioned preparation is added again in swimming pool, the amount added in water per ton is 3g, from bottom, air is filled with to it, aeration 15min, uses this degradable controlled release Scale inhibitors, wall and bottom do not have fouling, and water body keeps clean simultaneously.

Claims (1)

1. a preparation method for degradable controlled release Scale inhibitors, is characterized in that concrete preparation process is:

(1) 1:5 in mass ratio, maleic acid is added in deionized water, and be placed in four-hole boiling flask, be dissolved in completely after in deionized water at 70 ~ 80 DEG C of heating in water bath to maleic acid subsequently, continue Heat preservation 10 ~ 15min, stop subsequently heating and making it naturally cool to 20 ~ 25 DEG C, be prepared into maleic acid solution;

(2) 1:2 in mass ratio, by mass concentration be 25% ammonia soln be added in maleic acid solution, be heated to 80 ~ 90 DEG C subsequently, make its stirring reaction 3 ~ 5h, be prepared into transparent glass liquid, subsequently glass precursor solution be placed in air dry oven, dry 1 ~ 2h at 160 ~ 180 DEG C, cyclodehydration 3 ~ 4h in 210 ~ 230 DEG C of vacuum dehumidifying devices, is prepared into yellow solid subsequently;

(3) 1:10 in mass ratio, the yellow solid of above-mentioned preparation is added in distilled water, after being heated to 50 ~ 60 DEG C subsequently, with the sodium hydroxide solution titration hydrolysis 1 ~ 2h of 0.5mol/L, after solution changes color to reddish-brown, stop heating making its naturally cooling and leave standstill 1 ~ 2h, it filtered and collects filtrate;

(4) 1:2 in mass ratio, the filtrate of collection is added in anhydrous methanol, subsequently under rotating speed 600 ~ 800r/min, make its Precipitation, after 45 ~ 60min to be mixed, staticly settle and to its filter, collect filtrate and to its rotary evaporation to original volume 1/3, be placed in 50 ~ 60 DEG C of baking ovens dry subsequently, be prepared into particle Scale inhibitors for subsequent use;

(5) 1:5 in mass ratio, gelatin is dissolved in distilled water at 55 ~ 60 DEG C, be uniformly mixed 10 ~ 15min and be prepared into gelatin solution, count by weight subsequently, choose the particle Scale inhibitors of the above-mentioned preparation of 30 ~ 45 parts, 10 ~ 15 parts 1, the gelatin solution of 4-butanediol diglycidyl ether and 45 ~ 55 parts, 30 ~ 45min is uniformly mixed at 600 ~ 800r/min, subsequently after standing and defoaming 2 ~ 3h, be placed in stainless steel mould, under 2 ~ 3MPa, lucifuge drying 4 ~ 5 days, can be prepared into degradable controlled release Scale inhibitors.