CN107758882B - Concentrated scale inhibition and dispersion agent for high sulfate and carbonate and preparation method thereof - Google Patents

Concentrated scale inhibition and dispersion agent for high sulfate and carbonate and preparation method thereof Download PDF

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CN107758882B
CN107758882B CN201711052799.9A CN201711052799A CN107758882B CN 107758882 B CN107758882 B CN 107758882B CN 201711052799 A CN201711052799 A CN 201711052799A CN 107758882 B CN107758882 B CN 107758882B
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scale inhibition
water
dispersion agent
acid
carbonate
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CN107758882A (en
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潘兴灿
王冬生
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Shandong Ludong Environment Tech Co ltd
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
    • C02F5/14—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • 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
    • C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
    • C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
    • C02F5/12—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing nitrogen

Abstract

The invention relates to a concentrated scale inhibition and dispersion agent for high sulfate and carbonate and a preparation method thereof, and the concentrated scale inhibition and dispersion agent comprises the following components: acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer, phosphonocarboxylic acid copolymer, diethylenetriamine pentamethylene phosphoric acid, 1, 1-diphosphonic acid sodium propionate phosphonate, polyaspartic acid, hexamethylenediamine tetramethylidene phosphonate potassium salt and water. The invention discloses a concentrated scale inhibition and dispersion agent for high sulfate and carbonate, which is prepared by compounding six components of AA-AMPS, POCA, DTPMPA and the like for the first time, the concentrated scale inhibition and dispersion agent has good scale inhibition and dispersion effects on water with high sulfate radical, high barium and strontium content, does not cause secondary pollution to a membrane system, has very strong scale inhibition effect on high calcium magnesium ions, can remove old scales, has low adding concentration and low cost, and can achieve good scale inhibition and dispersion effects generally at 0.5-10 ppm.

Description

Concentrated scale inhibition and dispersion agent for high sulfate and carbonate and preparation method thereof
Technical Field
The invention relates to a concentrated scale inhibition and dispersion agent for high sulfate and carbonate and a preparation method thereof, belonging to the technical field of chemical scale inhibitors.
Background
In the most serious historical period of environmental pollution in China, the national department of environmental protection is accelerating to make a thirteen-five plan of environmental protection and implement three ten plans of atmosphere, water and soil. Thirteen five plans propose to promote water pollution treatment comprehensively, complete a second sewage treatment and reclaimed water utilization three-year action scheme comprehensively, insist on centralized and decentralized combination, pollutant interception and pollution control coordination, perfect promotion of water quality purification technology, accelerate the construction of water treatment facilities, basically realize the full collection and full treatment of urban and rural water, and improve the urban and rural sewage treatment rate to more than 95%. Meanwhile, the construction of a water-saving society is strived to insist on saving priority in the future, and a resource view of saving, intensive recycling is established. The strictest water resource management system is implemented, the water is used for fixed production, the water is used for fixed city, and a water-saving society is built.
Due to the trouble of the water crisis, the water recycling of all countries in the world is more and more important, and the recycling technology is widely applied to the countries of Japan, America, Israel and the like. With the emphasis of China on energy conservation and emission reduction, the effective utilization rate of reclaimed water after sewage treatment is more and more concerned, and the requirement on the advanced treatment capacity of recycled water is more and more great. At present, most factories try to adopt a zero emission concept that sewage does not leave factories to repeatedly utilize industrial drainage. Wherein, the sewage of the circulating water can enter a reverse osmosis system for filtration through the processes of lime sedimentation, flocculation precipitation, ultrafiltration and the like. The filtered pure water can be used for supplementing water to the circulating water, so that a part of fresh water is saved, and the concentrated water further enters an evaporator and other equipment for evaporation and desalination. Thereby achieving the purpose of zero-emission water saving.
The sewage of the circulating water is concentrated by several times in the running process of the circulating water system and contains higher salts such as carbonate, sulfate, iron ions and the like. In particular, in some factories with high alkalinity and high hardness water quality, in order to save water and increase the concentration multiple of circulating water, the traditional method of adding sulfuric acid to control pH value, which is low in cost and high in efficiency, is generally adopted according to the recommendation of the Ministry of construction, "control standard of circulating water management". This sulfuric acid-adjusted pH circulating water will contain a significant amount of sulfate ions. Sulfate scale formation is often encountered during use in reverse osmosis further filtration. And sulfate scale is well known to be very difficult to wash, once generated, is difficult to remove, often causes the blockage of a reverse osmosis membrane, reduces the water production performance, and wastes the membrane in advance, thereby greatly increasing the operation cost of enterprises.
The scale inhibitor existing in the current market has no ideal effect on scale inhibition and dispersion with sulfate, and the market has a higher share of imported brands such as several medicaments of Narkii and Japanese chestnut fields in the United states.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a concentrated scale inhibition and dispersion agent which is compatible with a reverse osmosis membrane, a nanofiltration membrane and an ultrafiltration membrane and aims at high sulfate and carbonate and a preparation method thereof.
The invention is realized by the following technical scheme:
a concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS): 30-35%;
phosphonocarboxylic acid copolymer (POCA): 15-20%;
diethylenetriamine penta (methylene phosphate DTPMPA): 15% -20%;
sodium 1, 1-diphosphopropionate phosphonate (BPBP): 15 to 20 percent;
polyaspartic Acid (PASP): 10-20%;
hexamethylenediamine tetramethylphosphonic acid potassium salt (hdtmpa. k 6): 5-10%;
water: and (4) the balance.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS) in percentage by weight: 30%, 31%, 32%, 33%, 34% or 35%.
According to the invention, the concentrated scale inhibiting and dispersing agent for high sulfate and carbonate comprises phosphono carboxylic acid copolymer (POCA) in weight percentage: 15%, 16%, 17%, 18%, 19% or 20%.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight: 15%, 16%, 17%, 18%, 19% or 20%.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight (BPBP): 20%, 21%, 22%, 23%, 24% or 25%.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises Polyaspartic Acid (PASP) in percentage by weight: 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight: 5%, 6%, 7%, 8%, 9% or 10%.
According to the invention, the concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS): 35 percent;
phosphonocarboxylic acid copolymer (POCA): 18 percent;
diethylenetriamine penta (methylene phosphate DTPMPA): 15 percent;
sodium 1, 1-diphosphopropionate phosphonate (BPBP): 15 percent;
polyaspartic Acid (PASP): 10 percent;
hexamethylenediamine tetramethylphosphonic acid potassium salt (hdtmpa. k 6): 7 percent.
A preparation method of a concentrated scale inhibition and dispersion agent aiming at high sulfate and carbonate comprises the following steps:
(1) adding acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS), phosphono carboxylic acid copolymer (POCA) and diethylenetriamine pentamethylene phosphoric acid (DTPMPA) in proportion under the conditions of water as a solvent, normal temperature and pressure and stirring at the rotating speed of 100-200 r/min to prepare an acidic raw material mixture;
(2) adding alkaline raw materials of potassium hexamethylenediamine tetramine phosphate (HDTMPA. K6), sodium 1-1 diphosphonate propionylphosphonate (BPBP) and Polyaspartic Acid (PASP) into the acidic raw material mixture prepared in the step (1) to prepare a mixed raw material;
(3) and (3) increasing the rotating speed of the mixed raw material prepared in the step (2) to 200-300 r/min, stirring for 25-35 minutes, and cooling to normal temperature to obtain the composite material.
Advantageous effects
1. The invention discloses a concentrated scale inhibition and dispersion agent for high sulfate and carbonate, which is prepared by compounding six components of AA-AMPS, POCA, DTPMPA and the like for the first time, the concentrated scale inhibition and dispersion agent has good scale inhibition and dispersion effects on high sulfate radical, high barium and strontium water in water, does not cause secondary pollution to a membrane system, has very strong scale inhibition effect on high calcium magnesium ions, can remove old scale, has low adding concentration and low cost, and can achieve good scale inhibition and dispersion effects generally at 0.5-10 ppm;
2. the concentrated scale inhibition and dispersion agent can be compatible with various flocculants such as polyaluminium chloride, cationic polyacrylamide, ST polymeric flocculant and the like, and can effectively control CaCO3、CaSO4、BaSO4And SrSO4And FeO scaling, can realize that the L.S.I value is up to 3.5 and no scaling is generated;
3. the concentrated scale inhibition and dispersion agent can effectively control CaSO4The concentration product reaches 6 times, and the Fe at the concentrated water side can be realized<The coating normally plays a role under the concentration of 5mg/L, and the application range is wider;
drawings
FIG. 1 is a process flow diagram for recycling saponified wastewater generated in the production of propylene oxide by a chlorohydrination method used in Experimental example 2;
FIG. 2 is a graph of water pressure, total pressure differential, water production flow and water production conductance after use of an embodiment of the present invention with a prior art product;
Detailed Description
The technical solution of the present invention is further described with reference to the following examples, but the scope of the present invention is not limited thereto.
Source of raw materials
Acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS): weifang's Jinshi is environment-friendly, and is used in Pasteur, Dow;
phosphonocarboxylic acid (POCA) was purchased from: jujube zhuangtai and water treatment limited;
polyaspartic Acid (PASP) purchased: purchased from: jujube zhuangtai and water treatment limited;
diethylenetriamine penta (methylene phosphate) (DTPMPA) is purchased from: jujube zhuangtai and water treatment limited, a source of fresh water in the south of the river;
sodium 1, 1-diphosphonate propionylphosphonate (BPBP) was purchased from Pasf, Zizhuangtai, and Water treatment, Inc., USA;
potassium salt of hexanediamine tetra methylene phosphonate (hdtmpa. k6) was purchased from juzhuangtai and water treatment limited, source of fresh water in south of the river;
example 1
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000031
a preparation method of a concentrated scale inhibition and dispersion agent aiming at high sulfate and carbonate comprises the following steps:
(1) under the stirring conditions of water as a solvent, normal temperature and pressure and a rotating speed of 100-200 r/min, adding acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS), phosphono carboxylic acid copolymer (POCA) and diethylenetriamine pentamethylene phosphoric acid (DTPMPA) in proportion to prepare an acidic raw material mixture;
(2) adding alkaline raw materials of potassium hexamethylenediamine tetramine phosphate (HDTMPA. K6), sodium 1-1 diphosphonate propionylphosphonate (BPBP) and Polyaspartic Acid (PASP) into the acidic raw material mixture prepared in the step (1) to prepare a mixed raw material;
(3) and (3) increasing the rotating speed of the mixed raw material prepared in the step (2) to 200-300 r/min, stirring for 25-35 minutes, and cooling to normal temperature and normal pressure to obtain the composite material.
Example 2
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000041
the preparation method is the same as example 1.
Example 3
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000042
the preparation method is the same as example 1.
Example 4
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000043
the preparation method is the same as example 1.
Example 5
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000051
the preparation method is the same as example 1.
Example 6
A concentrated scale inhibition and dispersion agent for high sulfate and carbonate comprises the following components in percentage by weight:
Figure BDA0001451996220000052
the preparation method is the same as example 1.
Comparative example 1
The scale inhibition and dispersion agent comprises the following components in percentage by weight:
Figure BDA0001451996220000053
the preparation method is the same as example 1.
Comparative example 2
The scale inhibition and dispersion agent comprises the following components in percentage by weight:
Figure BDA0001451996220000054
Figure BDA0001451996220000061
the preparation method is the same as example 1.
Comparative example 3
The scale inhibition and dispersion agent comprises the following components in percentage by weight:
Figure BDA0001451996220000062
the preparation method is the same as example 1.
Test example 1
Experimental method for testing performance of scale inhibitor
The calcium carbonate resistance experiment refers to a calcium carbonate deposition method for determining the performance of the scale inhibitor for water treatment according to the national standard GB/T16632-2008 of the people's republic of China. The calcium phosphate and barium sulfate experiments refer to the enterprise standard Q/SYTZ0177-2007 of China oil and gas Limited.
CaCO-resistant3Scale experiments
Preparing 500mL of scale inhibitor and Ca with a certain concentration by using deionized water2+、HCO3 -Adjusting pH, placing in constant temperature water bath, keeping at a certain temperature for a certain period of time, cooling, measuring Ca with 0.22m microporous filter by EDTA method2+And (5) carrying out a blank test at the same time.
CaSO4 scale inhibition experiment
Preparing 500mL of scale inhibitor and Ca with a certain concentration by using deionized water2+、SO4 2-Adjusting pH, placing in constant temperature water bath, keeping at a certain temperature for a certain period of time, cooling, measuring Ca with 0.22m microporous filter by EDTA method2+And (5) carrying out a blank test at the same time.
Experiment for inhibiting BaSO4 scale
Preparing 500mL of scale inhibitor and Ba with a certain concentration by using deionized water2+、SO4 2-Adjusting pH, placing in constant temperature water bath, keeping the temperature at a certain temperature for a certain period of time, cooling, measuring Ba with 0.22m microporous filter by ion emission spectrometry2+And (5) carrying out a blank test at the same time.
SrSO4 scale inhibition experiment
500mL of scale inhibitor and Sr with certain concentration are prepared by deionized water2+、SO4 2-Adjusting pH, placing in constant temperature water bath, keeping the temperature at a certain temperature for a certain period of time, cooling, filtering with 0.22m microporous filter, and separatingDetermination of Sr by using sub-emission spectrometry2+And (5) carrying out a blank test at the same time.
Results of the experiment
The scale inhibition and dispersion experiments were carried out by the methods described above using the high sulfate carbonate concentrated scale inhibition and dispersion agents prepared in examples 1 and 2 and comparative examples 1, 2, and 3, and the results are shown in table 1. As can be seen from Table 1, the products of examples 1 and 2 of the present invention are more effective in controlling CaCO3 and CaSO4BaSO4 and SrSO4, and particularly has a very significant scale inhibition effect on sulfates.
TABLE 1
Figure BDA0001451996220000071
Test example 2
Dynamic field tracking experiment
Overview of the treated Water System: the method is used for treating the Propylene Oxide (PO) wastewater, and the Propylene Oxide (PO) is a third large propylene derivative which is second to polypropylene and acrylonitrile, is widely applied to industries such as petroleum, chemical industry, pesticides, textile, daily chemicals and the like, and is an important basic organic chemical raw material. At present, the capacity of producing the propylene oxide by the chlorohydrin method accounts for 51 percent of the total production capacity of the world, and the method is the most classical method for producing the propylene oxide in China. 50-80 tons of wastewater can be generated in the production of 1 ton of propylene oxide by a chlorohydrination method, and the wastewater has the advantages of high pH value, high salt content, high COD (chemical oxygen demand) and CaCl2High concentration, low biodegradability and the like, and is difficult to treat, thus becoming the primary factor restricting the industrial development of the propylene oxide.
At present, few researches on the treatment of PO production wastewater by a chlorohydrin method are carried out at home and abroad, and the research is mostly focused on a microbial method. However, since the PO wastewater is treated in the process, Ca (OH) in the wastewater2Is easy to react with CO in the air2Calcium carbonate crystals are generated by reaction, so that the suspended matters in the pretreated wastewater exceed the standard, and the subsequent biochemical treatment effect is influenced; meanwhile, the salinity of the wastewater is high, general microorganisms are difficult to adapt, and the general microbial method is not suitable for treating the high-salinity wastewater.
In the experiment, the effects of different medicaments are analyzed and compared by selecting the embodiment 4 and the embodiment 6, comparing the embodiment with the embodiment 3 and the inlet medicament and detecting the changes of pressure, pressure difference, conductivity and water yield in the operation process after the operation is carried out for a period of time, and the optimal medicament suitable for the system is selected.
The water quality condition is as follows:
as shown in Table 2, the water was high in calcium ion concentration, sulfate ion concentration, carbonate ion content, bicarbonate ion content, silicon ion content, and fluoride ion content. The water is easy to scale in the reverse osmosis concentration process, so the performance requirement on the scale inhibitor is very strict.
TABLE 2
Inspection item Unit of Numerical value Inspection item Unit of Numerical value
pH ___ 6.5-9.5 Dissolved Solids (TDS) mg/L 35000
Na+ mg/L 100 Total hardness (in Ca) mg/L 12000
k+ mg/L 20 Total alkalinity mg/L 80
Ca2+ mg/L 12000 Suspended matter mg/L 10
Mg2+ mg/L 30 all-Silicon (SiO)2) mg/L 0.008
Total nitrogen mg/L 10 Active Silicon (SiO)2) mg/L 0.003
Ammonia nitrogen mg/L 1 Silicon rubber (SiO)2) mg/L 0.005
Total phosphorus (in PO)4 9) mg/L 1.5 CODcr mg/L 100
CL- mg/L 22000 BOD5 mg/L 20
SO4 2- mg/L 100 Color intensity Dilution factor 20
NO3 - mg/L 200 Turbidity of water NTU 5
TOC mg/L 80 Fecal coliform group Per L 100
The treatment process comprises the following steps: the treatment is carried out according to the process flow chart recorded in figure 1, wherein 1 in figure 1 is propylene oxide wastewater; 2. a primary sedimentation tank; 3. a sedimentation tank; 4. treating flue gas; 5. the peripheral section ph of the metering pump; 6. a sand filter; 7. a plate heat exchanger; 8. an ultrafiltration unit; 9. raw water RO; 10. RO of concentrated water; 11. recycling reverse osmosis produced water; 12. concentrated water RO concentrated water; 13. second-stage RO concentrated water; 14. a calcium oxide evaporation tower; 15. calcium chloride crystallization recovery; 16. recycling distilled water of the distillation tower; 17. sludge treatment;
wherein the reverse osmosis membrane adopts three membrane components of Dow XC-70, XC-80 and HPRO.
And (3) test results: the detection results of the water quality tracking records are shown in table 3, and the detection results of the system operation data are shown in table 4;
TABLE 3 Water quality Trace record
Figure BDA0001451996220000081
Figure BDA0001451996220000091
Table 4: reverse osmosis plant operational data tracking
Figure BDA0001451996220000092
By comparing and analyzing the loss rates of ions in the reverse osmosis influent and concentrate water qualities in table 3, it can be seen that the loss rates of examples 4, 5, and 6 are much lower than those of comparative examples 1, 2, and 3. This shows that examples 4, 5 and 6 have a good stabilizing effect in the presence of high sulfate radical, high calcium ion and high silicon ion, and are less likely to form scale and to prevent membrane clogging.
According to the field use data in table 4, the operation pressure difference, the salt rejection rate and the water inlet pressure of the equipment using the embodiments 4, 5 and 6 of the invention are more stable. The scale inhibition of the example 4 is stable, and far exceeds the scale inhibition effect of an imported product 5200 of Nalrco in America, as shown in figure 2.

Claims (2)

1. A concentrated scale inhibition and dispersion agent for high sulfate and carbonate is characterized by comprising the following components in percentage by weight:
carboxylate-sulfonate-nonionic terpolymer: 35 percent;
phosphonoacrylic acid: 15 percent;
polyaspartic acid: 10 percent;
diethylenetriamine pentamethylene phosphoric acid: 20 percent;
1, 1-diphospho propionic acid radical sodium phosphonate: 15 percent;
hexamethylenediamine tetramethylidene phosphonic acid potassium salt: 5 percent;
water: the balance;
the high sulfate and carbonate are dissolved solids values of 35000mg/L, and total hardness values in terms of Ca are 12000 mg/L; the dosing concentration is 5 ppm.
2. The preparation method of the concentrated scale inhibition and dispersion agent for high sulfate and carbonate according to claim 1 is characterized by comprising the following steps:
(1) adding acrylic acid-2-acrylamide-2-methylpropanesulfonic acid copolymer (AA-AMPS), phosphono carboxylic acid copolymer (POCA) and diethylenetriamine pentamethylene phosphoric acid (DTPMPA) in proportion under the conditions of water as a solvent, normal temperature and pressure and stirring at the rotating speed of 100-200 r/min to prepare an acidic raw material mixture;
(2) adding alkaline raw materials of potassium hexamethylenediamine tetramethylidene phosphonate (HDTMPA. K6), sodium 1-1 diphosphonate propionylphosphonate (BPBP) and Polyaspartic Acid (PASP) into the acidic raw material mixture prepared in the step (1) to prepare a mixed raw material;
(3) and (3) increasing the rotating speed of the mixed raw material prepared in the step (2) to 200-300 r/min, stirring for 25-35 minutes, and cooling to normal temperature to obtain the composite material.
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