CN112593234A - Preparation method of ammonium citrate - Google Patents
Preparation method of ammonium citrate Download PDFInfo
- Publication number
- CN112593234A CN112593234A CN202011404653.8A CN202011404653A CN112593234A CN 112593234 A CN112593234 A CN 112593234A CN 202011404653 A CN202011404653 A CN 202011404653A CN 112593234 A CN112593234 A CN 112593234A
- Authority
- CN
- China
- Prior art keywords
- ammonium citrate
- prepared
- flame retardant
- stirrer
- putting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 105
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003063 flame retardant Substances 0.000 claims abstract description 44
- 238000000227 grinding Methods 0.000 claims abstract description 33
- 239000004696 Poly ether ether ketone Substances 0.000 claims abstract description 31
- 229920002530 polyetherether ketone Polymers 0.000 claims abstract description 31
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 31
- 239000013543 active substance Substances 0.000 claims abstract description 30
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 239000003755 preservative agent Substances 0.000 claims abstract description 24
- 230000002335 preservative effect Effects 0.000 claims abstract description 24
- 239000007800 oxidant agent Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004595 color masterbatch Substances 0.000 claims abstract description 16
- 230000001590 oxidative effect Effects 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 12
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- -1 polyethylene Polymers 0.000 claims description 7
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 238000005915 ammonolysis reaction Methods 0.000 claims description 6
- 239000003822 epoxy resin Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- 229920000647 polyepoxide Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 239000012258 stirred mixture Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 13
- 238000005260 corrosion Methods 0.000 abstract description 13
- 239000003086 colorant Substances 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000011363 dried mixture Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000013556 antirust agent Substances 0.000 description 1
- 239000006172 buffering agent Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003516 soil conditioner Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000001393 triammonium citrate Substances 0.000 description 1
- 235000011046 triammonium citrate Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
Abstract
The invention discloses a preparation method of ammonium citrate, in particular to the technical field of ammonium citrate, and the technical scheme is as follows: the preparation method comprises the following preparation steps: s1, purchasing citric acid, water, liquid ammonia, a preservative, a flame retardant, an oxidant, polyether ether ketone, polyurethane resin, color master, a dispersing agent, an active agent and an accelerant, and selecting qualified products after purchasing; s2, sequentially and separately putting the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein the preparation method of the ammonium citrate has the beneficial effects that: by adding the preservative, the flame retardant, the polyether-ether-ketone, the polyurethane resin, the color master batch and the dispersing agent in a proper proportion, the corrosion resistance, the flame retardant performance and the high and low temperature resistance of the ammonium citrate can be improved, and the ammonium citrate can have various colors.
Description
Technical Field
The invention relates to the technical field of ammonium citrate, and particularly relates to a preparation method of ammonium citrate.
Background
Ammonium citrate, also called triammonium citrate, is white deliquescent powder or crystal, is easy to dissolve in water, is decomposed at the melting point and has low toxicity, and is mainly used for chemical analysis, industrial water treatment, metal cleaning, ceramic dispersing agent, permeation aid, detergent raw material and soil conditioner components, and also used in the industries of medicine, electronics and the like, and is used as a chemical reagent in analytical chemistry, such as determination of phosphate in fertilizer, determination of phosphate and effective phosphoric acid in fertilizer, and is used as a cyanide-free electroplating complexing agent in electroplating industry, and is used as an antirust agent in mechanical industry, and is used as a buffering agent, an emulsifying agent and the like in food industry, and is obtained by the action of citric acid and ammonia water.
The prior art has the following defects: when the existing ammonium citrate is used as a rust inhibitor in the mechanical industry, the corrosion resistance, the flame retardant property and the high and low temperature resistance of the existing ammonium citrate are poor, and the color of the existing ammonium citrate is single, so that the service life of the existing ammonium citrate is shortened, and the sales volume of the existing ammonium citrate is reduced.
Therefore, the invention is necessary to develop a preparation method of ammonium citrate.
Disclosure of Invention
Therefore, the invention provides a preparation method of ammonium citrate, which is characterized in that a preservative, a flame retardant, polyether-ether-ketone, polyurethane resin, color master and a dispersing agent are added in a proper proportion during proportioning, so that the corrosion resistance, the flame retardant property and the high and low temperature resistance of the ammonium citrate can be improved, the ammonium citrate can have various colors, and the problems that the existing ammonium citrate is poor in corrosion resistance, flame retardant property and high and low temperature resistance and single in color are solved.
In order to achieve the above purpose, the invention provides the following technical scheme: the preparation method comprises the following preparation steps:
s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerator into a grinding machine for grinding, and separately placing the obtained powder after grinding;
s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;
s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;
s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying and drying the mixture after cooling and crystallizing, and putting the mixture into a grinder for grinding to obtain the product.
Preferably, in S2, after the flame retardant, the polyether ether ketone, the polyurethane resin, the activator, and the accelerator are ground, the grinding machine needs to be cleaned to grind the next material.
Preferably, in S7, the cooled and crystallized mixture is placed into a dryer for drying.
Preferably, the material of the preservative is water-based epoxy resin.
Preferably, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.
Preferably, the oxidizing agent is potassium dichromate and concentrated sulfuric acid according to the ratio of 1: 1 ratio of the components.
Preferably, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.
Preferably, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 1: 1 ratio of the components.
Preferably, the accelerator is provided as accelerator ZDC.
The invention has the beneficial effects that:
according to the invention, citric acid, water and liquid ammonia are selected as main materials, and the preservative with a proper proportion is added in the proportioning process, so that the corrosion resistance of ammonium citrate is greatly improved, the service life of ammonium citrate can be prolonged, then the flame retardant with a proper proportion is added, so that the flame retardant property of ammonium citrate can be effectively improved, the ammonium citrate can not be softened and ignited when used at high temperature, and the polyether-ether-ketone with a proper proportion is added, so that the high and low temperature resistance of ammonium citrate is improved, the corrosion resistance of ammonium citrate is also improved, meanwhile, the polyurethane resin with a proper proportion is added, so that the corrosion resistance of ammonium citrate is improved, the ammonium citrate has the characteristics of high strength, tear resistance and wear resistance, the applicability is improved, and the color master batch and the dispersant with a proper proportion are added, this gives ammonium citrate a variety of colors and thus increases sales.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1:
the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:
s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether-ether-ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerant into a grinding machine for grinding, and separately putting obtained powder after grinding, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerant, the grinding machine needs to be cleaned, so that the next material can be ground;
s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;
s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;
s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.
Furthermore, the material of the preservative is aqueous epoxy resin.
Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.
Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 1 ratio of the components.
Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.
Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 1: 1 ratio of the components.
Further, the accelerator is provided as accelerator ZDC.
Example 2:
the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:
s1, purchasing 60g of citric acid, 80g of water, 30g of liquid ammonia, 5g of preservative, 6g of flame retardant, 4g of oxidant, 5g of polyether-ether-ketone, 8g of polyurethane resin, 4g of color master batch, 2g of dispersant, 2g of active agent and 4g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 6g of flame retardant, 5g of polyether-ether-ketone, 8g of polyurethane resin, 2g of active agent and 4g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, and then the next material can be ground;
s3, pouring 80g of water and 60g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;
s4, heating the citric acid aqueous solution to 50 ℃, and then ammonolyzing the citric acid aqueous solution by 30g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer with the temperature of 100 ℃, adding 5g of preservative and 6g of flame retardant, stirring for 3min, adding 4g of oxidant, 5g of polyether-ether-ketone and 8g of polyurethane resin, and stirring for 5 min;
s6, cooling the temperature of the stirrer to 80 ℃, after cooling, putting 2g of the active agent and 4g of the accelerant into the stirrer to be stirred for 3min, then cooling the temperature of the stirrer to 50 ℃, and then putting 4g of the color master batch and 2g of the dispersing agent into the stirrer to be stirred for 4 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.
Furthermore, the material of the preservative is aqueous epoxy resin.
Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 1 ratio of the components.
Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 0.3 proportion.
Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.4: 1 ratio of the components.
Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 0.5: 1 ratio of the components.
Further, the accelerator is provided as accelerator ZDC.
Example 3:
the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:
s1, purchasing 70g of citric acid, 90g of water, 40g of liquid ammonia, 7.5g of preservative, 8g of flame retardant, 5g of oxidant, 7.5g of polyether-ether-ketone, 10g of polyurethane resin, 5g of color master batch, 3g of dispersing agent, 3g of active agent and 6g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 8g of flame retardant, 7.5g of polyether-ether-ketone, 10g of polyurethane resin, 3g of active agent and 6g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, so that the next material can be ground;
s3, pouring 90g of water and 70g of citric acid into a mixer for mixing, thereby obtaining an aqueous citric acid solution;
s4, heating the citric acid aqueous solution to 65 ℃, and then ammonolyzing the citric acid aqueous solution by 40g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer with the temperature of 105 ℃, firstly adding 7.5g of preservative, 8g of flame retardant and 5g of oxidant, then stirring for 2min, then adding 7.5g of polyether-ether-ketone and 10g of polyurethane resin, and stirring for 6.5 min;
s6, cooling the temperature of the stirrer to 82.5 ℃, then putting 5g of color master batch and 3g of dispersing agent into the stirrer to be stirred for 3.5min, cooling the temperature of the stirrer to 55 ℃ after cooling, and then putting 3g of active agent and 6g of accelerant into the stirrer to be stirred for 5 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.
Furthermore, the material of the preservative is aqueous epoxy resin.
Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 0.6: 1 ratio of the components.
Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 0.5: 1 ratio of the components.
Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.7: 1 ratio of the components.
Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 0.6: 1 ratio of the components.
Further, the accelerator is provided as accelerator ZDC.
Example 4:
the invention provides a preparation method of ammonium citrate, which comprises the following preparation steps:
s1, purchasing 80g of citric acid, 100g of water, 50g of liquid ammonia, 10g of preservative, 10g of flame retardant, 6g of oxidant, 10g of polyether-ether-ketone, 12g of polyurethane resin, 6g of color master batch, 4g of dispersing agent, 4g of active agent and 8g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 10g of flame retardant, 10g of polyether-ether-ketone, 12g of polyurethane resin, 4g of active agent and 8g of accelerator into a grinding machine for grinding, and after grinding, separately putting the obtained powder, wherein after grinding the flame retardant, the polyether-ether-ketone, the polyurethane resin, the active agent and the accelerator, the grinding machine needs to be cleaned, and then the next material can be ground;
s3, pouring 100g of water and 80g of citric acid into a stirrer to mix, thereby obtaining an aqueous citric acid solution;
s4, heating the citric acid aqueous solution to 80 ℃, and then ammonolyzing the citric acid aqueous solution by 50g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer at the temperature of 110 ℃, sequentially adding 10g of preservative, 10g of flame retardant, 6g of oxidant and 10g of polyether-ether-ketone, stirring for 6min, adding 12g of polyurethane resin, and stirring for 8 min;
s6, cooling the temperature of the stirrer to 85 ℃, after cooling, putting 4g of active agent and 8g of accelerant into the stirrer to be stirred for 5min, then cooling the temperature of the stirrer to 60 ℃, and then putting 6g of color master batch and 4g of dispersing agent into the stirrer to be stirred for 6 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying the mixture in a dryer after cooling and crystallizing, and crushing the dried mixture in a crusher to obtain the product.
Furthermore, the material of the preservative is aqueous epoxy resin.
Further, the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 0.8: 1 ratio of the components.
Further, the oxidizing agent is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 0.7: 1 ratio of the components.
Further, the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 1: 2 in proportion.
Further, the active agent is a mixture of diphenylguanidine and zinc oxide in a ratio of 3: 1 ratio of the components.
Further, the accelerator is provided as accelerator ZDC.
The ammonium citrates prepared in examples 1 to 4 above were compared to obtain the following data:
as can be seen from the above table, the ammonium citrate prepared in examples 1 to 4 has better performance in terms of corrosion resistance, flame retardancy, high and low temperature resistance, color and life, but the ammonium citrate has different effects in terms of corrosion resistance, flame retardancy, high and low temperature resistance, color and life because the ratio of citric acid to water to liquid ammonia to preservative to flame retardant to oxidant to polyether ether ketone to polyurethane resin to color master batch to dispersant to activator to accelerator is different, wherein: citric acid, water and liquid ammonia are used as main materials, and a proper proportion of preservative is added in the proportioning process, so that the corrosion resistance of the ammonium citrate is greatly improved, the service life of the ammonium citrate can be prolonged, then a proper proportion of flame retardant is added, the flame retardant performance of the ammonium citrate can be effectively improved, the ammonium citrate can not be softened and ignited when used at high temperature, and a proper proportion of polyether-ether-ketone is added, so that the high and low temperature resistance of the ammonium citrate is improved, the corrosion resistance of the ammonium citrate is also improved, meanwhile, a proper proportion of polyurethane resin is added, the corrosion resistance of the ammonium citrate is improved, the ammonium citrate has the characteristics of high strength, tear resistance and wear resistance, the applicability is improved, and the color master batch and the dispersant are added in proper proportion, so that the ammonium citrate has multiple colors, therefore, the sales volume can be increased, after the coating is used, the effect of the embodiment 4 is optimal, various colors are kept while the corrosion resistance, the flame retardant property and the high and low temperature resistance are improved, the service life is prolonged, and the application range is enlarged.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the present invention or modify it into an equivalent technical solution by using the technical solution described above. Therefore, any simple modifications or equivalent substitutions made in accordance with the technical solution of the present invention are within the scope of the claims of the present invention.
Claims (9)
1. A preparation method of ammonium citrate is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
s1, purchasing 60g-80g of citric acid, 80g-100g of water, 30g-50g of liquid ammonia, 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 4g-6g of color master batch, 2g-4g of dispersing agent, 2g-4g of active agent and 4g-8g of accelerant, and selecting qualified products after purchasing;
s2, sequentially and separately putting 6g-10g of flame retardant, 5g-10g of polyether ether ketone, 8g-12g of polyurethane resin, 2g-4g of active agent and 4g-8g of accelerator into a grinding machine for grinding, and separately placing the obtained powder after grinding;
s3, pouring 80g-100g of water and 60g-80g of citric acid into a stirrer for mixing, thereby obtaining a citric acid aqueous solution;
s4, heating the citric acid aqueous solution to 50-80 ℃, and then aminolyzing the citric acid aqueous solution by 30-50 g of liquid ammonia;
s5, putting the solution after ammonolysis into a stirrer with the temperature of 100-110 ℃, and then adding 5g-10g of preservative, 6g-10g of flame retardant, 4g-6g of oxidant, 5g-10g of polyether ether ketone and 8g-12g of polyurethane resin in sequence for stirring for 5-8 min;
s6, cooling the temperature of the stirrer to 80-85 ℃, after cooling, putting 2-4 g of active agent and 4-8 g of accelerant into the stirrer to be stirred for 3-5min, then cooling the temperature of the stirrer to 50-60 ℃, and then putting 4-6 g of color master batch and 2-4 g of dispersing agent into the stirrer to be stirred for 4-6 min;
and S7, taking out the stirred mixture, cooling and crystallizing, drying and drying the mixture after cooling and crystallizing, and putting the mixture into a grinder for grinding to obtain the product.
2. The method of claim 1, wherein the ammonium citrate is prepared by: in S2, after the flame retardant, the polyether ether ketone, the polyurethane resin, the activator, and the accelerator are ground, the grinding machine needs to be cleaned to grind the next material.
3. The method of claim 1, wherein the ammonium citrate is prepared by: and S7, putting the cooled and crystallized mixture into a dryer for drying.
4. The method of claim 1, wherein the ammonium citrate is prepared by: the preservative is made of water-based epoxy resin.
5. The method of claim 1, wherein the ammonium citrate is prepared by: the flame retardant is prepared from antimony trioxide and zinc borate according to the weight ratio of 1: 0.5 proportion.
6. The method of claim 1, wherein the ammonium citrate is prepared by: the oxidant is prepared from potassium dichromate and concentrated sulfuric acid according to the weight ratio of 1: 1 ratio of the components.
7. The method of claim 1, wherein the ammonium citrate is prepared by: the dispersing agent is prepared from polyethylene low molecular wax and stearate according to the weight ratio of 0.5: 1 ratio of the components.
8. The method of claim 1, wherein the ammonium citrate is prepared by: the active agent is a mixture of diphenyl guanidine and zinc oxide according to the ratio of 1: 1 ratio of the components.
9. The method of claim 1, wherein the ammonium citrate is prepared by: the accelerator is set to accelerator ZDC.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011404653.8A CN112593234A (en) | 2020-12-03 | 2020-12-03 | Preparation method of ammonium citrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011404653.8A CN112593234A (en) | 2020-12-03 | 2020-12-03 | Preparation method of ammonium citrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112593234A true CN112593234A (en) | 2021-04-02 |
Family
ID=75188155
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011404653.8A Pending CN112593234A (en) | 2020-12-03 | 2020-12-03 | Preparation method of ammonium citrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112593234A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250100A (en) * | 2021-12-30 | 2022-03-29 | 湖北图致新材料科技有限公司 | Lubricating oil formula optimized based on high polymer material and preparation process thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0432610A2 (en) * | 1989-12-11 | 1991-06-19 | Innova S.A. | Concurrent production of citric acid and alkali citrates |
| CN1389449A (en) * | 2002-07-16 | 2003-01-08 | 南通恒兴电子材料有限公司 | Electron-level ammonium citrate and its production process |
| CN1424299A (en) * | 2002-12-20 | 2003-06-18 | 杨春明 | Ammonium citrate preparation |
| CN101654409A (en) * | 2009-08-12 | 2010-02-24 | 广东光华化学厂有限公司 | Divalent coloring metal citric acid ammonium salt and preparation method and application thereof |
| CN103159615A (en) * | 2011-12-13 | 2013-06-19 | 李月平 | Ammonium citrate synthesizing method |
| CN106854151A (en) * | 2015-12-08 | 2017-06-16 | 中粮生物化学（安徽）股份有限公司 | The production method of Triammonium citrate crystal and the Triammonium citrate crystal produced by the method |
-
2020
- 2020-12-03 CN CN202011404653.8A patent/CN112593234A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0432610A2 (en) * | 1989-12-11 | 1991-06-19 | Innova S.A. | Concurrent production of citric acid and alkali citrates |
| CN1389449A (en) * | 2002-07-16 | 2003-01-08 | 南通恒兴电子材料有限公司 | Electron-level ammonium citrate and its production process |
| CN1424299A (en) * | 2002-12-20 | 2003-06-18 | 杨春明 | Ammonium citrate preparation |
| CN101654409A (en) * | 2009-08-12 | 2010-02-24 | 广东光华化学厂有限公司 | Divalent coloring metal citric acid ammonium salt and preparation method and application thereof |
| CN103159615A (en) * | 2011-12-13 | 2013-06-19 | 李月平 | Ammonium citrate synthesizing method |
| CN106854151A (en) * | 2015-12-08 | 2017-06-16 | 中粮生物化学（安徽）股份有限公司 | The production method of Triammonium citrate crystal and the Triammonium citrate crystal produced by the method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250100A (en) * | 2021-12-30 | 2022-03-29 | 湖北图致新材料科技有限公司 | Lubricating oil formula optimized based on high polymer material and preparation process thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2531564B1 (en) | A process for the preparation of carbon black pellets | |
| EP2870121B1 (en) | Process for preparing an emulsion of elemental sulphur particles | |
| CN1692154B (en) | Method for the production of a solid fragrance concentrate | |
| CN107352839A (en) | A kind of gunite concrete liquid alkali-free chlorine-free accelerator and preparation method thereof | |
| EP0507402B1 (en) | Process for preparing detergent compositions | |
| CN112593234A (en) | Preparation method of ammonium citrate | |
| CN108793111A (en) | A kind of method and products thereof of quick preparation phosphatization cobalt | |
| US6476082B1 (en) | Magnesium ammonium phosphate hexahydrate slurry | |
| CN102442735B (en) | Method for treating wastewater of rubber antioxidant (RD) production device | |
| GB1562399A (en) | Stable fluid suspension fertilizer composition and method for prducing same | |
| US4185066A (en) | Method of treating magnesium oxchloride and magnesium oxysulfate articles to reduce efflorescence | |
| US3416910A (en) | Method of preventing reversion to citrate insoluble form | |
| CN106277477A (en) | The processing method of acid-bearing wastewater in a kind of 2,4 diamino benzene sulfonic acids and salt production process thereof | |
| US3645797A (en) | Metal phosphatizing composition and process | |
| DE10360819A1 (en) | Glass granulate material, is formed by preparing an aqueous glass binder, adding glass powder, stirring, adding more powder, drying and foaming | |
| US718537A (en) | Bordeaux mixture and method of making same. | |
| CN109748610A (en) | A kind of water-soluble fertilizer and production method that the residual fertilizer of the medicine that can degrade is residual | |
| US11820656B2 (en) | Preparation method for water-soluble potassium polymetaphosphate | |
| US2776205A (en) | Iron-fluorine compound | |
| AU684923B2 (en) | Non-aqueous neutralization of N-acyl sarcosines | |
| CN107686123A (en) | A kind of solid liquid interface fast preparation method of cuprous bromide crystal thin-film material | |
| JPH0475017B2 (en) | ||
| JPS61242635A (en) | Composition retarded in reactivity or dissolubility with water or acid and alkali aqueous solution and its production | |
| JP2015000365A (en) | Powdery fire-extinction chemical-treatment substance, and manufacturing method therefor | |
| JPH10194882A (en) | Granular fertilizer composition, liquid fertilizer composition, pasty fertilizer composition and their production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210402 |
|
| RJ01 | Rejection of invention patent application after publication |