CN108545842A - A kind of preparation method of the preparation method of novel green antisludging agent - Google Patents
A kind of preparation method of the preparation method of novel green antisludging agent Download PDFInfo
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- CN108545842A CN108545842A CN201810434324.4A CN201810434324A CN108545842A CN 108545842 A CN108545842 A CN 108545842A CN 201810434324 A CN201810434324 A CN 201810434324A CN 108545842 A CN108545842 A CN 108545842A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- CQOVPNPJLQNMDC-ZETCQYMHSA-N carnosine Chemical compound [NH3+]CCC(=O)N[C@H](C([O-])=O)CC1=CNC=N1 CQOVPNPJLQNMDC-ZETCQYMHSA-N 0.000 claims abstract description 21
- 108010087806 Carnosine Proteins 0.000 claims abstract description 20
- CQOVPNPJLQNMDC-UHFFFAOYSA-N N-beta-alanyl-L-histidine Natural products NCCC(=O)NC(C(O)=O)CC1=CN=CN1 CQOVPNPJLQNMDC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 108010064470 polyaspartate Proteins 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims abstract description 18
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000012265 solid product Substances 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229920001577 copolymer Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006396 nitration reaction Methods 0.000 claims description 4
- 235000012216 bentonite Nutrition 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- -1 lauryl amines Chemical class 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- AISMNBXOJRHCIA-UHFFFAOYSA-N trimethylazanium;bromide Chemical compound Br.CN(C)C AISMNBXOJRHCIA-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 101710134784 Agnoprotein Proteins 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 238000013459 approach Methods 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 125000004888 n-propyl amino group Chemical class [H]N(*)C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000008247 solid mixture Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 206010013786 Dry skin Diseases 0.000 claims 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 206010042674 Swelling Diseases 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 239000000919 ceramic Substances 0.000 claims 1
- 238000005485 electric heating Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 230000008961 swelling Effects 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 5
- 230000002401 inhibitory effect Effects 0.000 abstract description 4
- 238000012546 transfer Methods 0.000 abstract description 4
- 229940044199 carnosine Drugs 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000007142 ring opening reaction Methods 0.000 abstract description 2
- QRYRORQUOLYVBU-VBKZILBWSA-N Carnosic acid Natural products CC([C@@H]1CC2)(C)CCC[C@]1(C(O)=O)C1=C2C=C(C(C)C)C(O)=C1O QRYRORQUOLYVBU-VBKZILBWSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 230000005764 inhibitory process Effects 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000002455 scale inhibitor Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 241001677188 Coccus viridis Species 0.000 description 2
- HNDVDQJCIGZPNO-YFKPBYRVSA-N L-histidine Chemical compound OC(=O)[C@@H](N)CC1=CN=CN1 HNDVDQJCIGZPNO-YFKPBYRVSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- UCMIRNVEIXFBKS-UHFFFAOYSA-N beta-alanine Chemical compound NCCC(O)=O UCMIRNVEIXFBKS-UHFFFAOYSA-N 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 239000001506 calcium phosphate Substances 0.000 description 2
- 229910000389 calcium phosphate Inorganic materials 0.000 description 2
- 235000011010 calcium phosphates Nutrition 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229920000578 graft copolymer Polymers 0.000 description 2
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 2
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical group [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 2
- 239000008235 industrial water Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 2
- 108010016626 Dipeptides Proteins 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920000805 Polyaspartic acid Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229940024606 amino acid Drugs 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229940000635 beta-alanine Drugs 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 229960002885 histidine Drugs 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- DCEMCPAKSGRHCN-UHFFFAOYSA-N oxirane-2,3-dicarboxylic acid Chemical compound OC(=O)C1OC1C(O)=O DCEMCPAKSGRHCN-UHFFFAOYSA-N 0.000 description 1
- 239000003348 petrochemical agent Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
Classifications
-
- 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
- C02F5/125—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 combined with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Detergent Compositions (AREA)
Abstract
The invention discloses a kind of preparation methods of novel green antisludging agent, and with maleic anhydride, urea, L carnosines etc. for raw material, poly-aspartate carnosine is prepared by ring-opening reaction, add adobe isomery material and obtain novel green antisludging agent.Antisludging agent scale-inhibiting properties prepared by the present invention are good, can be adsorbed on the Active Growth site of dirty crystal leads to crystal transfer or distortion of lattice, to destroy the normal growth of dirty crystal, inorganic salts in petrochemical industry and power process can effectively be inhibited to deposit scale problems in equipment surface.
Description
Technical field
The present invention relates to a kind of preparation methods of novel green antisludging agent, belong to industrial water conditioning agent design field.
Background technology
Recirculated cooling water occupies very big proportion in industrial water, and in recirculated cooling water operational process, water intermediate ion is dense
Degree is continuously improved, and the difficulty soluble salts such as calcium carbonate, calcium sulfate and calcium phosphate are deposited on metal surface, the heat exchange efficiency drop of metal device
It is low!And be subject to corrode, cause the device cycle of operation to shorten, expense increase, equipment scrapping can be also caused when serious.It is cold recycling
But it is the most frequently used and effective method that antisludging agent and corrosion inhibiter are added in water.
The development of antisludging agent mainly experienced polyphosphoric acid salt, organic phospho acid salt, acrylic acid and maleic acid polymers class,
And poly-epoxy succinic acid and the biodegradable class antisludging agent of polyaspartic acid.Preceding two classes antisludging agent is phosphorous, and facile hydrolysis causes
Body eutrophication causes a degree of pollution to environment.Acrylic acid derives from petrochemicals, with rise of the oil price,
Such antisludging agent cost Continued is non-biodegradation although polyacrylie-type and poly type antisludging agent be not phosphorous
Type.As mankind's environmental consciousness increasingly improves, environmental legislation and standard are increasingly stringent, exploitation it is low-phosphorous or without phosphorus, efficient, can biology
The green scale inhibitor of degradation becomes a hot spot in antisludging agent research and development field.It is original with maleic anhydride, urea, N-BETA-Alanyl-L-histidine etc.
Material, prepares poly-aspartate-carnosine by ring-opening reaction, adds adobe isomery material and obtain novel green antisludging agent,
Antisludging agent, which can be adsorbed on the Active Growth site of dirty crystal, leads to crystal transfer or distortion of lattice, to destroy dirty crystal
Normal growth can effectively inhibit inorganic salts in petrochemical industry and power process to deposit scale problems in equipment surface.
Invention content
The purpose of the present invention is to provide a kind of preparation method of novel green antisludging agent, which can be adsorbed on dirty crystalline substance
Lead to crystal transfer or distortion of lattice on the Active Growth site of body, to destroy the normal growth of dirty crystal, effectively maintains
The normal operation of industrial equipment.
A kind of preparation method of the preparation method of novel green antisludging agent, it is characterised in that this approach includes the following steps:
1）9.8 parts by weight maleic anhydrides are weighed in reaction kettle, 60 DEG C of dissolvings are heated to after 10 parts by weight distilled water are added,
4.2 parts by weight of urea reaction 1h is added after being warming up to 80 DEG C, 0.82 parts by weight nitration mixture is added dropwise after being continuously heating to 160 DEG C to be catalyzed
Dehydration is dehydrated 2h within the temperature range of 160 ~ 180 DEG C；Obtained solid is transferred in Buchner funnel very after stopping heating
Sky filters, and finally drying for 24 hours, obtains solid product in vacuum drying chamber；
2）The above-mentioned solid product of 5 parts by weight is taken to be scattered in 15 parts by weight distilled water, 0.5 parts by weight mass fraction, which is slowly added dropwise, is
30% NaOH solution is warming up to 60 DEG C, and reaction is for 24 hours；Use the hydrochloric acid solution that mass fraction is 10% by its pH tune after completion of the reaction
To 7 or so, 200 parts by weight absolute ethyl alcohols are then added, skims supernatant after standing 12h after magnetic agitation 30min, is dried in vacuo
Obtain poly-aspartate product；It weighs 0.3 ~ 0.7 parts by weight poly-aspartate and 0.4 ~ 0.8 parts by weight N-BETA-Alanyl-L-histidine is dissolved in 5 weight
In part distilled water, 0.25 parts by weight NaOH is added dropwise, is warming up to 60 DEG C, reaction is for 24 hours.PH value of solution is adjusted to hydrochloric acid after completion of the reaction
7 or so, 2 parts by weight adobe isomery materials are added, adds 60 parts by weight absolute ethyl alcohols, is stood after magnetic agitation 30min
Supernatant is skimmed after 12h, is dried in vacuo 12h, is obtained new copolymer antisludging agent.
Advantageous effect：The present invention is with maleic anhydride, urea, N-BETA-Alanyl-L-histidine etc. for a kind of novel green scale inhibition of Material synthesis
Agent, N-BETA-Alanyl-L-histidine are the dipeptides of two kinds of amino acid of Beta-alanine and L-Histidine composition, have preferable biological degradability, N-BETA-Alanyl-L-histidine
In the imidazoles heteroaromatic that contains can effectively adsorb calcium phosphate crystal, draw by the graft copolymer antisludging agent of Material synthesis of N-BETA-Alanyl-L-histidine
After entering carboxyl and imidazole group, the adsorption capacity of calcium ion is greatly improved, the conjugated system and N contained in copolymer antisludging agent
Antisludging agent can be improved to Ca in atom3（PO4）2The adsorption capacity of nucleus and sequestering power to calcium ion, and antisludging agent can be adsorbed on
Lead to dirty crystal transfer or distortion of lattice on the Active Growth site of dirty crystal, destroy the normal growth of dirty crystal, makes dirty crystalline substance
Body can not be perfectly adhered to instrument surface to more easily washed away.
Specific implementation mode
Embodiment 1
1）9.8 parts by weight maleic anhydrides are weighed in reaction kettle, 60 DEG C of dissolvings are heated to after 10 parts by weight distilled water are added,
4.2 parts by weight of urea reaction 1h is added after being warming up to 80 DEG C, 0.82 parts by weight nitration mixture is added dropwise after being continuously heating to 160 DEG C to be catalyzed
Dehydration is dehydrated 2h within the temperature range of 160 ~ 180 DEG C；Obtained solid is transferred in Buchner funnel very after stopping heating
Sky filters, and finally drying for 24 hours, obtains solid product in vacuum drying chamber；
2）The above-mentioned solid product of 5 parts by weight is taken to be scattered in 15 parts by weight distilled water, 0.5 parts by weight mass fraction, which is slowly added dropwise, is
30% NaOH solution is warming up to 60 DEG C, and reaction is for 24 hours；Use the hydrochloric acid solution that mass fraction is 10% by its pH tune after completion of the reaction
To 7 or so, 200 parts by weight absolute ethyl alcohols are then added, skims supernatant after standing 12h after magnetic agitation 30min, is dried in vacuo
Obtain poly-aspartate product；It weighs 0.4 parts by weight poly-aspartate and 0.7 parts by weight N-BETA-Alanyl-L-histidine is dissolved in 5 parts by weight distilled water
In, 0.25 parts by weight NaOH is added dropwise, is warming up to 60 DEG C, reaction is for 24 hours.PH value of solution is adjusted to 7 or so with hydrochloric acid after completion of the reaction, is added
Enter 2 parts by weight adobe isomery materials, adds 60 parts by weight absolute ethyl alcohols, skimmed after standing 12h after magnetic agitation 30min
Supernatant is dried in vacuo 12h, obtains new copolymer antisludging agent.
Above-mentioned adobe isomery material preparation method is as follows：
Take 4 bromide/cetyl of 100 parts by weight calcium-base bentonites and a concentration of 0.104mol/L of 1000 parts by weight
Trimethylammonium bromide（4 bromide/cetyl trimethylammonium bromide molar ratio is 1:2）Aqueous solution is sufficiently mixed, and is placed in
In constant temperature oscillator, reaction 2h is to ensure that absorption reaches balance under 60 DEG C and 50r/min；It is freezed after reaction using high speed
Centrifuge 4000r/min centrifuges 15min, is used in combination distilled water to rinse repeatedly to remove the 4 bromide and hexadecane that do not exchange
Base trimethylammonium bromide, until AgNO is added dropwise in filtrate3Without Br-Detection；Solid mixture obtained is placed in drying box 100 DEG C
Left and right is dry for 24 hours, then grinds, after sieving with 100 mesh sieve, takes 5 parts by weight of bentonite and 6 parts by weight n-propylamines, 6 parts by weight 12
Amine, 80 parts by weight acetoacetic esters are stirred to react 4 h in 60 DEG C after evenly mixing；Filtered on buchner funnel, solid part are used after the completion of reaction
It is stood overnight in locellus warm air, lower 550 DEG C of nitrogen state is made more with 3 DEG C/min temperature-programmed calcinations, 6 h in high temperature furnace
Hole clay isomery material.
Embodiment 2
Identical with embodiment 1, difference is：0.3 parts by weight poly-aspartate, 0.8 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 3
Identical with embodiment 1, difference is：0.35 parts by weight poly-aspartate, 0.75 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 4
Identical with embodiment 1, difference is：0.45 parts by weight poly-aspartate, 0.65 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 5
Identical with embodiment 1, difference is：0.5 parts by weight poly-aspartate, 0.6 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 6
Identical with embodiment 1, difference is：0.55 parts by weight poly-aspartate, 0.65 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 7
Identical with embodiment 1, difference is：0.6 parts by weight poly-aspartate, 0.5 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 8
Identical with embodiment 1, difference is：0.65 parts by weight poly-aspartate, 0.45 parts by weight N-BETA-Alanyl-L-histidine is added.
Embodiment 9
Identical with embodiment 1, difference is：0.7 parts by weight poly-aspartate, 0.4 parts by weight N-BETA-Alanyl-L-histidine is added.
Comparative example 1
Identical with embodiment 1, difference is：Only it is added without adobe isomery material.
Comparative example 2
Identical with embodiment 1, difference is：It is added without 4 bromide when only preparing adobe isomery material.
Comparative example 3
Identical with embodiment 1, difference is：It is added without cetyl trimethyl when only preparing adobe isomery material
Ammonium bromide.
Comparative example 4
Identical with embodiment 1, difference is：When only preparing adobe isomery material not under nitrogen state.
Comparative example 5
Identical with embodiment 1, difference is：Maleic anhydride is substituted for 2- hexyls -3- when only preparing antisludging agent
Methyl-maleic acid acid anhydride.
Comparative example 6
Identical with embodiment 1, difference is：It is added without N-BETA-Alanyl-L-histidine when only preparing antisludging agent.
Comparative example 7
Identical with embodiment 1, difference is：Reaction temperature is adjusted to 50 DEG C when only preparing antisludging agent.
Comparative example 8
Identical with embodiment 1, difference is：PH is not adjusted when only preparing antisludging agent.
The antisludging agent prepared as follows with comparative example 1 ~ 8 to the embodiment of the present invention 1 ~ 9 is tested for the property：
Scale inhibitor performance evaluation is tested
Hinder Ca3（PO4）2Dirty performance is by method evaluation as defined in GB/T1576-2008.Configure ρ（Ca2+）= 400mg/L（With
CaCO3Meter）And ρ（PO4 3-）= 400mg/L（With Na3PO4Meter）Solution, be added 1mg/L graft copolymer antisludging agents, be placed in 80
10h is heated in DEG C water bath with thermostatic control, take out it is cooling after, take 20mL supernatant liquors, sequentially add sodium tetraborate, ascorbic acid and ammonium molybdate
Solution, develop the color after mixing 15min, absorbance when using 723N type spectrophotometer measurement 710nm wavelength, calculates scale inhibition effect
Rate, computational methods see below formula；
η=（A
0
-A
1
）/(A
0
-A
2
)×100%
Wherein η is scale inhibition performance, A0To be not added with antisludging agent, absorbance when not heating；A1For be added antisludging agent, heat 10h when
Absorbance；A2To be not added with antisludging agent, absorbance when 10h is heated.
Scale inhibitor performance evaluation result
As seen from the above table, embodiment 1 is i.e. as 0.4 parts by weight poly-aspartate of addition, 0.7 parts by weight N-BETA-Alanyl-L-histidine, 10 parts by weight N-
N-tert-butyl acrylamide, antisludging agent prepared by when 2 parts by weight adobe isomery material is to Ca3（PO4）2Solution scale inhibition performance is
97.54%, scale-inhibiting properties are best, and when changing poly-aspartate, N-BETA-Alanyl-L-histidine parts by weight, the different degrees of reduction of scale inhibition performance can
The poly-aspartate and N-BETA-Alanyl-L-histidine seen in embodiment 1 cooperate with scale effect best, and scale inhibition performance highest has unexpected technology
Effect.The addition of the explanation of comparative example 1 ~ 4 adobe isomery material and the selection of preparation condition are to antisludging agent scale-inhibiting properties shadow
Sound is larger, when comparative example 5 ~ 8 illustrates to prepare antisludging agent the selection of raw material and synthesis condition have to antisludging agent scale-inhibiting properties very big
Influence.
Claims (5)
1. a kind of preparation method of novel green antisludging agent, it is characterised in that this approach includes the following steps:
1）9.8 parts by weight maleic anhydrides are weighed in reaction kettle, 60 DEG C of dissolvings are heated to after 10 parts by weight distilled water are added,
4.2 parts by weight of urea reaction 1h is added after being warming up to 80 DEG C, 0.82 parts by weight nitration mixture is added dropwise after being continuously heating to 160 DEG C to be catalyzed
Dehydration is dehydrated 2h within the temperature range of 160 ~ 180 DEG C；Obtained solid is transferred in Buchner funnel very after stopping heating
Sky filters, and finally drying for 24 hours, obtains solid product in vacuum drying chamber；
2）The above-mentioned solid product of 5 parts by weight is taken to be scattered in 15 parts by weight distilled water, 0.5 parts by weight mass fraction, which is slowly added dropwise, is
30% NaOH solution is warming up to 60 DEG C, and reaction is for 24 hours；Use the hydrochloric acid solution that mass fraction is 10% by its pH tune after completion of the reaction
To 7 or so, 200 parts by weight absolute ethyl alcohols are then added, skims supernatant after standing 12h after magnetic agitation 30min, is dried in vacuo
Obtain poly-aspartate product；It weighs 0.3 ~ 0.7 parts by weight poly-aspartate and 0.4 ~ 0.8 parts by weight N-BETA-Alanyl-L-histidine is dissolved in 5 weight
In part distilled water, 0.25 parts by weight NaOH is added dropwise, is warming up to 60 DEG C, reaction is for 24 hours;
PH value of solution is adjusted to 7 or so with hydrochloric acid after completion of the reaction, 2 parts by weight adobe isomery materials are added, add 60 weights
Part absolute ethyl alcohol is measured, supernatant is skimmed after 12h is stood after magnetic agitation 30min, is dried in vacuo 12h, obtains new copolymer resistance
Dirty agent.
2. a kind of preparation method of the preparation method of novel green antisludging agent according to claim 1, it is characterised in that above-mentioned
Step 1）Middle reaction kettle is ceramic electric heating reaction kettle.
3. a kind of preparation method of the preparation method of novel green antisludging agent according to claim 1, it is characterised in that above-mentioned
Step 1）The phosphoric acid that middle nitration mixture is the sulfuric acid that mass fraction is 95% and mass fraction is 85% is by 1:1 volume ratio uniformly mixes.
4. a kind of preparation method of the preparation method of novel green antisludging agent according to claim 1, it is characterised in that above-mentioned
Mixing speed is 300 ~ 400r/min in step.
5. a kind of preparation method of novel green antisludging agent according to claim 1, it is characterised in that the adobe is different
Structure material preparation method is as follows：
Take 4 bromide/cetyl of 100 parts by weight calcium-base bentonites and a concentration of 0.104mol/L of 1000 parts by weight
Trimethylammonium bromide aqueous solution is sufficiently mixed, and is placed in constant temperature oscillator, and reaction 2h is to ensure to adsorb under 60 DEG C and 50r/min
Reach balance；Use high speed freezing centrifuge 4000r/min to centrifuge 15min after reaction, be used in combination distilled water to rinse repeatedly with
The 4 bromide and cetyl trimethylammonium bromide not exchanged are removed, until AgNO is added dropwise in filtrate3Without Br-Detection；System
The solid mixture obtained is placed in 100 DEG C or so dryings in drying box and for 24 hours, then grinds, and after sieving with 100 mesh sieve, takes 5 parts by weight swellings
Soil is stirred to react 4 h in 60 DEG C after evenly mixing with 6 parts by weight n-propylamines, 6 parts by weight lauryl amines, 80 parts by weight acetoacetic esters；Instead
Should after the completion of use filtered on buchner funnel, stand overnight in solid portion air at room temperature, in high temperature furnace lower 550 DEG C of nitrogen state with
Adobe isomery material is made in 3 DEG C/min temperature-programmed calcinations, 6 h.
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| CN109607832A (en) * | 2018-11-30 | 2019-04-12 | 中能化地大热能(湖北)有限责任公司 | A kind of polyaspartic acid scale inhibitor and preparation method thereof |
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