CN115140849A - Linear release type long-acting phosphorus-free scale inhibitor - Google Patents
Linear release type long-acting phosphorus-free scale inhibitor Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
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Abstract
The invention provides a linear release type solid scale inhibitor which has the characteristics of long acting, stability, environmental friendliness and the like. The scale inhibitor takes a silicon dioxide framework as a carrier, can continuously and stably release an effective component, namely polyboroxide complex anions, can combine calcium ions and magnesium ions to form amorphous flocs under certain environmental conditions, and is discharged through solid-liquid separation, so that the scale inhibitor can realize the increase of the water concentration multiple without the increase of the concentrations of the calcium ions and the magnesium ions in water. The scale inhibitor is a solid inorganic phosphorus-free scale inhibitor, can keep the effective components in water at constant concentration by controlling the release rate, can continuously combine calcium ions and magnesium ions for a long time, cannot cause water quality deterioration, and has no eutrophication risk in drainage.
Description
Technical Field
The invention belongs to the field of water treatment agents, and relates to preparation and application of a linear release inorganic phosphorus-free scale inhibitor.
Background
Increasing the concentration multiple is an effective method for reducing the consumption of circulating water, but the concentration of calcium, magnesium and other ions in water is increased, so that the serious scaling problem is caused. The heat resistance of the scale is about 40-50 times that of carbon steel, and the scale can block the pipeline, thereby threatening the production safety. In order to effectively control the formation of these inorganic precipitates, scale inhibitors of the equivalent polyphosphate, phosphonate and polycarboxylate types have emerged.
US 09108866 and CN 102674571 disclose a series of amino acid alkyl phosphonic acid scale inhibitors based on threshold amounts, providing an effective scale control method using essentially a single active scale inhibitor. CN 109126474 describes a composite phosphorus-free scale inhibitor consisting of a dendrimer, sodium polyepoxysuccinate, sodium polyaspartate, IA-AMPS and water. CN 101700937 discloses a composite scale inhibitor suitable for high-hardness high-alkali industrial circulating water, which comprises HEDP, polyaspartic acid, polymaleic anhydride, polyacrylic acid dispersant and the like. CN 110066033, the corrosion and scale inhibitor composition contains maleic anhydride-allyloxy polyoxyethylene maleic acid monoester copolymer, organic phosphine compound, non-phosphate organic acid and/or non-phosphate organic acid salt, water soluble inorganic zinc salt, etc.
The mechanism of action of the phosphate/phosphonate is a threshold effect, preventing/inhibiting/delaying the formation of scale-like crystallites. The mode of operation of polycarboxylates is a lattice distortion and dispersion effect that prevents further growth of scale crystallites by adsorbing to the crystal surfaces of the scale and inhibiting the deposition and adhesion of scale on solid surfaces such as pipes and vessels. The forms can realize effective scale inhibition under certain concentration multiple, and are bound with larger water replenishing amount and water discharging amount. If the concentration multiple is continuously increased, the concentration of calcium and magnesium ions is inevitably increased, and the continuous concentration finally exceeds the scale inhibition capacity range.
In order to realize a continuous scale inhibition effect, the traditional liquid or instant scale inhibitor needs to be periodically added, and the concentration of effective scale inhibitor components in a circulating water system is periodically changed along with the addition of the traditional liquid or instant scale inhibitor. The scale inhibitor has scaling risk under the condition of low concentration and has no long-term effect. And the addition of the organic phosphorus-containing scale inhibitor enables the water body to be suitable for the growth of microorganisms, and biological slime is easily formed, so that thermal resistance of dirt and microbial corrosion are generated. In addition, discharge of concentrated water into natural water bodies can cause eutrophication problems.
Disclosure of Invention
Based on the background, the invention prepares a linear release type long-acting phosphorus-free scale inhibitor. In the present invention, silica and other raw materials are calcined and formed in one step by a melt calcination method. Forming an amorphous material with a silica framework loaded with polyborate. The slow linear release of the active ingredient is achieved by utilizing the tight combination of the silicon dioxide skeleton and the polyborate. When the polyborate reaches a certain concentration in the circulating water system, it will form polyboroxy complex anions, and flexible flocs are formed by combining calcium ions and magnesium ions. Finally, the sediment is discharged through solid-liquid separation, so that the concentration of calcium and magnesium ions in the circulating water system is always kept at a lower level and is not increased along with the increase of the concentration multiple.
The first aspect of the present invention is to maintain the concentration of active ingredient in a circulating water system at a constant value by using a one-step shaped silica matrix to deliver boron oxygen complex anions to achieve linear release of the active ingredient.
The second aspect of the invention is to utilize inorganic and phosphorus-free boron-oxygen anion complexes to realize self-assembly from bottom to top by sharing the vertexes of calcium and magnesium ions, form flexible fiber (network, flocculent) amorphous substances, discharge the substances in a precipitation mode and prevent the formation of crystals such as carbonate.
The third aspect of the invention provides a preparation method of a linear release type long-acting phosphorus-free scale inhibitor, which comprises the following steps:
step 1: weighing SiO 2 Powder, H 3 BO 3 、NaB 4 O 7 ·10H 2 O, grinding, mixing, sieving to remove large-particle SiO 2 And dried in an oven to remove free moisture.
Wherein, siO 2 The mass of (A) is 7.4-22.2g; h 3 BO 3 The mass of (b) is 15.08-47.31g; naB 4 O 7 ·10H 2 The mass of O is 15.01-48.03g; naHCO 2 3 The mass of (A) is 3-9g.
Step 2: and (3) raising the temperature of the muffle furnace to 500-1200 ℃, quickly putting the raw materials into the muffle furnace, preserving the temperature for 0.5-2.5h, and simultaneously preheating the die.
And step 3: and taking the molten product out of the reverse mold immediately, and naturally cooling and forming.
The fourth aspect of the invention is to provide the use of the material in the aspect of active ingredient linear release and scale inhibition.
Wherein, the liquid in the release rate determination experiment is pure water, and the water temperature is more than or equal to 30 ℃; in the scale inhibition performance test, the liquid environment contains 0-500mg/L of calcium ions and 0-500mg/L of magnesium ions, and the scale inhibition temperature is 30 ℃.
The invention has the following beneficial effects:
the scale inhibitors of the present invention utilize a silica backbone to deliver boron oxygen complex anions to achieve linear release of active ingredients. The active ingredient can be released linearly over a period of several months, maintaining the concentration of active ingredient in the circulating water system at a constant value. When the boron-oxygen complex anion reaches a certain concentration in a circulating water system, the boron-oxygen complex anion realizes self-assembly from bottom to top by sharing the vertexes of calcium and magnesium ions to form flexible fiber (network, flocculent) objects and inhibit the attachment, nucleation and growth of carbonate scale crystals on the surface of a pipeline. Finally, through solid-liquid separation, the calcium ion concentration in the circulating water system is always kept at a lower level and is not increased along with the increase of the concentration multiple, so that the high-efficiency scale inhibition under the condition of long-term high concentration multiple is realized.
Drawings
Fig. 1 shows the appearance of the linear release inorganic phosphorus-free scale inhibitor of the present invention;
FIG. 2 shows a 60-fold micrograph of amorphous flocs produced by calcium and magnesium ions in conjunction with boron-oxygen complex anions according to the present invention;
figure 3 shows the linear release profile of scale inhibitor 3 in example 3;
fig. 4 shows the removal performance curve of scale inhibitor 1 against calcium and magnesium ions in example 1;
fig. 5 shows the product composition structure of scale inhibitor 1 acting on calcium and magnesium ions in example 1.
Detailed Description
The materials and environments of use of the present invention are described in detail below for a part of exemplary embodiments, so that the skilled person can more clearly understand the embodiments. However, the following examples and descriptions are not intended to limit the present invention, and in the technical context of the present invention, different environments, different modifications, or other equivalent implementations may be used, and all of which are within the scope of the present invention. The scope of the invention is defined by the appended claims.
Example 1
The preparation method of the scale inhibitor 1 comprises the following steps:
weighing SiO 2 Powder 7.4g, H 3 BO 3 15.1g of powder, naB 4 O 7 ·10H 2 O powder 15.0g, naHCO 3 3.0g of powder, grinding, fully mixing, sieving to remove large-particle SiO 2 And drying the mixture in a vacuum drying oven at 80 ℃ for 2 hours to remove free moisture. And (3) raising the temperature of the muffle furnace to 1050 ℃, and quickly putting the raw materials into the muffle furnace for heat preservation for 1.5h. The graphite mold was heated to 120 ℃ for preheating, the molten product was immediately taken out and poured into the mold, and the mold was immediately capped to prevent the product from being cracked by quenching. And then naturally cooling and forming.
Linear release monitoring:
putting a certain volume of scale inhibitor 1 with a regular shape into pure water, wherein the dosage of the scale inhibitor is 800mg/L, sealing, putting into a 30 ℃ constant temperature oscillator, and periodically monitoring the total boron concentration in the water by using an inductively coupled plasma mass spectrometer.
Scale inhibition performance monitoring:
putting a certain volume of scale inhibitor 1 with a regular shape into a solution containing 300mg/L of calcium ions and 300mg/L of magnesium ions, wherein the dosage of the scale inhibitor is 5000mg/L. The solution is placed in a constant temperature oscillator at 30 ℃ for a linear release and scale inhibition experiment for 5.5 days, then 2-time, 4-time and 6-time concentration is carried out on the solution, the concentrations of calcium and magnesium ions in the solution are monitored by an inductively coupled plasma mass spectrometer after water samples are periodically taken and filtered, and the composition of a precipitation product is monitored by X-ray photoelectron spectroscopy.
And (3) testing results:
1. the linear release monitoring results are as follows:
TABLE 1-1 relationship of total boron concentration in solution as a function of release time
The results show that: the linear relation between the total boron concentration (y) in 30 days and the release time (x) is y =6.1906x +62.881, and the correlation coefficient R 2 =0.774. The release rate is about 23.51mg L in the initial 5.5d of the release period -1 d -1 Slow line in the range of 5.5-30 daysIn the sexual release stage, the release rate is about 3.59mg L -1 d -1 。
2. The scale inhibition performance monitoring results are as follows:
TABLE 1-2 calcium and magnesium ion concentrations as a function of time in the environment described in example 1
Tables 1-3 the concentration of calcium and magnesium ions as a function of the concentration factor in the environment described in example 1
The results show that the calcium ion concentration is gradually reduced and stabilized in the concentration range of 49-59 mg/L; the concentration of magnesium ions is gradually reduced and stabilized in the concentration range of 145-155 mg/L. The scale inhibitor 1 can continuously remove calcium and magnesium ions, so that the concentration of the calcium and magnesium ions is not increased along with the increase of the concentration multiple.
Example 2
The preparation method of the scale inhibitor 2 comprises the following steps:
weighing SiO 2 14.8g of powder H 3 BO 3 15.1g of powder, naB 4 O 7 ·10H 2 O powder 33.0g, naHCO 3 Powder 6.0g, the rest of the procedure is the same as in example 1.
Linear release monitoring:
the monitoring method was the same as in example 1.
Monitoring the scale inhibition performance:
the monitoring method was the same as in example 1.
And (3) testing results:
1. the linear release monitoring results were as follows:
TABLE 2-1 Total boron concentration in solution as a function of release time in the environment described in example 2
The results show that: the linear relation between the total boron concentration (y) in 30 days and the release time (x) is y =7.9306x +30.41, and the correlation coefficient R 2 =0.950. The release rate is approximately linear in 30 days and is about 8.01mg L -1 d -1 。
2. The scale inhibition performance monitoring results are as follows:
TABLE 2-2 calcium and magnesium ion concentrations as a function of time in the environment described in example 2
Tables 2-3 the concentration of calcium and magnesium ions as a function of the concentration factor in the environment described in example 2
The result shows that the concentration of calcium ions is gradually reduced and stabilized in the concentration range of 118-125 mg/L; the concentration of magnesium ions is gradually reduced and stabilized in the concentration range of 114-119 mg/L. The scale inhibitor 2 can continuously remove calcium and magnesium ions, so that the concentration of the calcium and magnesium ions is not increased along with the increase of the concentration multiple.
Example 3
The preparation method of the scale inhibitor 3 comprises the following steps:
weighing SiO 2 22.2g of powder H 3 BO 3 15.1g of powder, naB 4 O 7 ·10H 2 O powder 48.3g, naHCO 3 Powder 9.0g, the procedure is as in example 1.
Linear release monitoring:
the monitoring method was the same as in example 1.
Monitoring the scale inhibition performance:
the monitoring method was the same as in example 1.
Testing As a result:
1. the linear release monitoring results are as follows:
TABLE 3-1 Total boron concentration in solution as a function of release time in the environment described in example 3
The results show that: the linear relation between the total boron concentration (y) in 30 days and the release time (x) is y =6.1892x +16.457, and the correlation coefficient R 2 =0.994. The release rate is about 6.57mg L, and the release rate is linear within 30 days -1 d -1 。
2. The scale inhibition performance monitoring results are as follows:
TABLE 3-2 calcium and magnesium ion concentrations as a function of time in the environment described in example 3
Tables 3-3 the concentration of calcium and magnesium ions as a function of the concentration factor in the environment described in example 3
The results show that the calcium ion concentration is gradually reduced and stabilized in the concentration range of 104-116 mg/L; the magnesium ion concentration is gradually reduced and stabilized in the concentration range of 145-154 mg/L. The scale inhibitor 3 can continuously remove calcium and magnesium ions, so that the concentration of the calcium and magnesium ions is not increased along with the increase of the concentration multiple.
The above description is only for some embodiments of the present invention, but the protection scope of the present invention is not limited to the above cases, and the formulation modification or equivalent replacement in the background of the present invention should be included in the scope of the present invention.
Claims (10)
1. The linear release type long-acting phosphorus-free scale inhibitor is characterized by comprising silicon dioxide and polyborate, wherein the silicon dioxide is a carrier, and the polyborate is a precursor of an effective component.
2. The scale inhibitor according to claim 1, wherein the scale inhibitor is an inorganic phosphorus-free solid scale inhibitor, and the chemical structure is in an amorphous state.
3. The scale inhibitor according to claim 1, wherein the silica carrier is formed in one step by melt calcination, and the content of the silica carrier is 7-50%.
4. The scale inhibitor of claim 1, wherein the precursor is a polyborate having the formula:
X-Y
wherein X is an alkali metal cation, such as Na + Or K + (ii) a Y has the formula:
B a -O b wherein the atomic number ratio of boron (B) to oxygen (O) is a: B.
5. The precursor according to claim 4, wherein the raw materials for forming the precursor are orthoboric acid and alkali metal borate, wherein the proportion of orthoboric acid is 23% -74%, and the proportion of alkali metal borate is 26% -77%.
6. The scale inhibitor according to any one of claims 1 to 5, wherein the precursor raw material alkali metal borate is selected from at least one of sodium tetraborate (with or without crystal water) or potassium tetraborate (with or without crystal water).
7. The method for preparing the scale inhibitor according to any one of claims 1 to 6, characterized by comprising the steps of: weighing silicon dioxide powder, orthoboric acid, alkali metal borate and sodium bicarbonate, grinding, mixing uniformly, sieving to remove large-particle silicon dioxide, and drying in an oven to remove free moisture; heating a muffle furnace to 500-1200 ℃, quickly putting the raw materials into the muffle furnace, preserving heat for 0.5-2.5 hours, and preheating a mold; and immediately taking the molten product out of the reverse mold, and naturally cooling and molding.
8. The preparation method according to claim 7, wherein the mass ratio of the silica powder, orthoboric acid, alkali metal borate and sodium bicarbonate is 7.4-22.2.
9. Use of the scale inhibitor according to any one of claims 1 to 5 for scale inhibition in a liquid environment.
10. The application of the scale inhibitor in the aspect of claim 9, wherein the scale inhibitor is released in a liquid environment and the scale inhibiting temperature is more than or equal to 30 ℃; in the scale inhibition performance test, the initial liquid environment contains 0-500mg/L of calcium ions and 0-500mg/L of magnesium ions; the concentration multiple can be increased to 6 times, and the concentration of calcium and magnesium ions is not obviously increased.
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