CN113209914A - Preparation method of antimony pentoxide colloid for flame resistance of textile fabrics - Google Patents
Preparation method of antimony pentoxide colloid for flame resistance of textile fabrics Download PDFInfo
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- CN113209914A CN113209914A CN202110490638.8A CN202110490638A CN113209914A CN 113209914 A CN113209914 A CN 113209914A CN 202110490638 A CN202110490638 A CN 202110490638A CN 113209914 A CN113209914 A CN 113209914A
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- antimony pentoxide
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- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 title claims abstract description 181
- 239000000084 colloidal system Substances 0.000 title claims abstract description 25
- 239000004753 textile Substances 0.000 title claims abstract description 18
- 239000004744 fabric Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 18
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 16
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 14
- 239000004310 lactic acid Substances 0.000 claims abstract description 14
- 150000002978 peroxides Chemical class 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010992 reflux Methods 0.000 claims abstract description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 7
- 229910001414 potassium ion Inorganic materials 0.000 claims abstract description 5
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium superoxide Chemical compound [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 claims description 8
- 238000005342 ion exchange Methods 0.000 claims description 6
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 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 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 150000001463 antimony compounds Chemical class 0.000 description 1
- FAWGZAFXDJGWBB-UHFFFAOYSA-N antimony(3+) Chemical compound [Sb+3] FAWGZAFXDJGWBB-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0004—Preparation of sols
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/47—Oxides or hydroxides of elements of Groups 5 or 15 of the Periodic Table; Vanadates; Niobates; Tantalates; Arsenates; Antimonates; Bismuthates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Colloid Chemistry (AREA)
Abstract
The invention discloses a preparation method of antimony pentoxide colloid for flame retardance of textile fabrics, which comprises the steps of uniformly mixing antimony trioxide powder and peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 90-100 ℃ after dropwise adding, condensing, refluxing and stirring for 1-2 hours to obtain antimony pentoxide sol; heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 in a water bath at 95-100 ℃ until the water content is 40-45% to obtain antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring at room temperature for 2-5 h, and performing suction filtration to obtain modified antimony pentoxide sol; removing sodium ions or potassium ions in the antimony pentoxide sol in the step S2 at 30-35 ℃ by using cation exchange resin; heating the antimony pentoxide sol obtained in the step S3 at 95-98 ℃, evaporating, concentrating to 46-48%, adding lactic acid into the concentrated sol, stirring for 30-60 min, heating in a water bath at 50-70 ℃, dropwise adding an ethanol solution, and stirring for 1-2 h after dropwise adding to obtain the antimony pentoxide sol.
Description
Technical Field
The invention belongs to the technical field of antimony pentoxide colloid for flame retardance of textile fabrics, and particularly relates to a preparation method of antimony pentoxide colloid for flame retardance of textile fabrics.
Background
Antimony pentoxide colloid has many advantages such as large specific surface area, high thermal stability, strong covering power and transparency, so it has wide application. In addition, antimony pentoxide colloid has the characteristics of small particle size of 1-100 nm, high transparency, good thermal stability, low smoke generation amount, low toxicity and the like, and is widely used as a flame retardant for plastics, fibers and the like. The traditional method for preparing antimony pentoxide organosol can be roughly divided into two methods: direct and indirect processes. The direct method is to directly prepare antimony pentoxide organosol by using a trivalent antimony compound as a raw material and controlling certain conditions. US3657179 in anhydrous Sb2O5Or SbCl3Nitric acid is added and then heated, followed by the addition of the alpha hydroxy carboxylic acid, followed by an organic solvent (DMF), and finally the water is evaporated off.
Antimony pentoxide (Sb)2O5) And other antimony compounds, are widely used as flame retardant additives for flammable goods such as plastics, chemical fibers, rubber, cotton and linen fabrics, paint, copper-clad laminates and the like, and are used for preventing impurities such as nickel, vanadium, iron, copper and the like in petroleum from poisoning catalysts to reduce the recovery rate of the petroleum fraction when the catalyst is used for the petroleum fraction. However, in conventional applications, antimony pentoxide and the like are mainly incorporated in the form of a dry powder or a hydrosol insoluble in the system to be used. The powder is easy to aggregate and difficult to disperse, and precipitates are generated; the water-soluble antimony pentoxide colloidal solution has good dispersibility, but when used in an organic system, the water-soluble antimony pentoxide colloidal solution has poor oil-water miscibility, so that the phenomena of layering, foaming, emulsification and the like are caused, and the use effect is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of antimony pentoxide colloid for flame retardance of textiles, which comprises the following steps:
s1: and uniformly mixing antimony trioxide powder and peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 90-100 ℃ after dropwise adding, and carrying out condensation reflux stirring for 1-2 hours to obtain antimony pentoxide sol.
S2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 in a water bath at 95-100 ℃ until the water content is 40-45% to obtain antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring at room temperature for 2-5 h, and performing suction filtration to obtain the modified antimony pentoxide sol.
S3: and (4) removing sodium ions or potassium ions in the antimony pentoxide sol in the step S2 at 30-35 ℃ by using cation exchange resin, and keeping the pH value in the sol at 6.5-6.8 after ion exchange.
S4: heating the antimony pentoxide sol obtained in the step S3 at 95-98 ℃, evaporating, concentrating to 46-48%, adding lactic acid into the concentrated sol, stirring for 30-60 min, heating in a water bath at 50-70 ℃, dropwise adding an ethanol solution, and stirring for 1-2 h after dropwise adding to obtain the antimony pentoxide sol.
Further, the peroxide is any one of sodium peroxide or potassium peroxide.
Further, the mass ratio of the antimony trioxide powder to the peroxide is (1.55-1.75): (1-1.26).
Further, the mass ratio of the antimony trioxide powder to the triethylamine is (1-2) to (0.12-0.24).
Further, the mass-volume ratio of the antimony trioxide powder to the distilled water is (1-2) g (25-60) mL.
Further, the dropping rate of the distilled water in the step S1 is 0.15-0.20 mL/S, and the dropping is carried out for 6-10 min; then dropwise adding the mixture to the required solution amount at the dropwise adding rate of 0.36-0.4 mL/s.
Further, the cation exchange resin is selected from any one of cation exchange resin 001 × 7, cation exchange resin 201 × 7, cation exchange resin D001, and cation exchange resin D113.
Further, in the step S4, the amount of the added lactic acid is 8-15% of the sol in the step S3; the dripping rate of the ethanol is 0.2-0.35 mL/s, and the dripping time is 400-800 s.
Has the advantages that: in the invention, antimony trioxide powder and peroxide are uniformly mixed, then the mixture is added into a container, distilled water is dripped, and antimony pentoxide sol is obtained by condensation, reflux and stirring; heating, evaporating and concentrating to obtain antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, and performing suction filtration to obtain modified antimony pentoxide sol; removing sodium ions or potassium ions in the antimony pentoxide sol by using cation exchange resin; and heating, evaporating and concentrating again, adding lactic acid, stirring, heating in a water bath, and dropwise adding an ethanol solution to obtain the antimony pentoxide sol, wherein the obtained antimony pentoxide sol has good dispersibility, can be used in an organic system, and has an excellent light projection rate.
Detailed Description
The following embodiments of the present invention are described in detail, and the embodiments are implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, it should be noted that, for those skilled in the art, a plurality of modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
A preparation method of antimony pentoxide colloid for flame resistance of textile fabrics specifically comprises the following steps:
s1: uniformly mixing antimony trioxide powder and sodium peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 90 ℃ after dropwise adding, condensing, refluxing and stirring for 1h to obtain antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the peroxide is 1.55: 1; the dropping rate of the distilled water is 0.15mL/s, and the dropping is carried out for 6 min; then, the solution was added dropwise at a dropping rate of 0.36mL/s to the desired amount of the solution.
S2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 under the condition of a water bath at 95 ℃, until the water content is 40%, obtaining antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring for 2 hours at room temperature, and performing suction filtration to obtain the modified antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the triethylamine is 1:0.12, and the mass-volume ratio of the antimony trioxide powder to the distilled water is 1g:25 mL.
S3: the antimony pentoxide sol in step S2 was freed of sodium ions at 30 ℃ with a cation exchange resin 001X 7, and the pH in the sol after ion exchange was maintained at 6.5.
S4: heating the antimony pentoxide sol obtained in the step S3 at 95 ℃, evaporating, concentrating to 46%, adding lactic acid into the concentrated sol, stirring for 30min, heating in a water bath at 50 ℃, dropwise adding an ethanol solution, and stirring for 1h after dropwise adding to obtain the antimony pentoxide sol, wherein the amount of the added lactic acid is 8% of that of the sol obtained in the step S3; the dropping rate of the ethanol is 0.2mL/s, and the dropping time is 400 s.
Example 2
A preparation method of antimony pentoxide colloid for flame resistance of textile fabrics specifically comprises the following steps:
s1: uniformly mixing antimony trioxide powder and potassium peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 100 ℃ after dropwise adding, condensing, refluxing and stirring for 2 hours to obtain antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the peroxide is 1.75: 1.26; the dropping rate of the distilled water is 0.20mL/s, and the dropping time is 10 min; then, the solution was added dropwise at a dropping rate of 0.4mL/s to the desired amount of the solution.
S2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 under the condition of water bath at 100 ℃, obtaining antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring for 5 hours at room temperature, and performing suction filtration to obtain the modified antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the triethylamine is 2:0.24, and the mass-volume ratio of the antimony trioxide powder to the distilled water is 2g:60 mL.
S3: the antimony pentoxide sol in step S2 was freed from potassium ions at 35 ℃ by cation exchange resin 201X 7, and the pH in the sol after ion exchange was maintained at 6.8.
S4: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S3 to 48% at 98 ℃, adding lactic acid into the concentrated sol, stirring for 60min, then heating in a water bath at 70 ℃, dropwise adding an ethanol solution, and stirring for 2h after dropwise adding to obtain the antimony pentoxide sol, wherein the amount of the added lactic acid is 15% of that of the sol obtained in the step S3; the dropping rate of the ethanol is 0.35mL/s, and the dropping time is 800 s.
Example 3
A preparation method of antimony pentoxide colloid for flame resistance of textile fabrics specifically comprises the following steps:
s1: uniformly mixing antimony trioxide powder and sodium peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 95 ℃ after dropwise adding, condensing, refluxing and stirring for 1.5 hours to obtain antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the peroxide is 1.65: 1.16; the dropping rate of the distilled water is 0.17mL/s, and the dropping is carried out for 8 min; then, the solution was added dropwise at a dropping rate of 0.38mL/s to the desired amount of the solution.
S2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 under the condition of water bath at 98 ℃, obtaining antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring for 3 hours at room temperature, and performing suction filtration to obtain the modified antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to triethylamine is 1.5:0.18, and the mass-volume ratio of the antimony trioxide powder to distilled water is 1.4g:40 mL.
S3: the antimony pentoxide sol in step S2 was freed of sodium ions at 32 ℃ with cation exchange resin D001, and the pH in the sol after ion exchange was maintained at 6.6.
S4: heating the antimony pentoxide sol obtained in the step S3 at 96 ℃, evaporating, concentrating to 47%, adding lactic acid into the concentrated sol, stirring for 40min, heating in a water bath at 60 ℃, dropwise adding an ethanol solution, and stirring for 1.5h after the dropwise adding is finished to obtain the antimony pentoxide sol, wherein the amount of the added lactic acid is 10% of that of the sol obtained in the step S3; the dropping rate of the ethanol is 0.5mL/s, and the dropping time is 600 s.
Example 4
A preparation method of antimony pentoxide colloid for flame resistance of textile fabrics specifically comprises the following steps:
s1: uniformly mixing antimony trioxide powder and sodium peroxide or potassium peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 98 ℃ after dropwise adding, and carrying out condensation reflux stirring for 2 hours to obtain antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the peroxide is 1.72: 1.24; the dropping rate of the distilled water is 0.19mL/s, and the dropping time is 9 min; then, the solution was added dropwise at a dropping rate of 0.39mL/s to the desired amount of the solution.
S2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 under the condition of water bath at 98 ℃, obtaining antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring for 4 hours at room temperature, and performing suction filtration to obtain the modified antimony pentoxide sol, wherein the mass ratio of the antimony trioxide powder to the triethylamine is 1.8:0.22, and the mass-volume ratio of the antimony trioxide powder to the distilled water is 1.8g:50 mL.
S3: the antimony pentoxide sol in step S2 was freed of sodium ions at 34 ℃ by means of a cation exchange resin D113, and the pH of the sol after ion exchange was maintained at 6.7.
S4: heating the antimony pentoxide sol obtained in the step S3 at 97 ℃, evaporating, concentrating to 48%, adding lactic acid into the concentrated sol, stirring for 50min, heating in a water bath at 65 ℃, dropwise adding an ethanol solution, and stirring for 1h after the dropwise adding is finished to obtain the antimony pentoxide sol, wherein the amount of the added lactic acid is 12% of that of the sol obtained in the step S3; the dropping rate of the ethanol is 0.30mL/s, and the dropping time is 700 s.
And (3) performance testing: (1) light transmittance measurement-the antimony pentoxide colloid prepared in examples 1 to 4 was diluted with distilled water to 10 times the original volume, and the diluted hydrosol was placed in a glass cuvette and subjected to light transmittance measurement at 676nm using a spectrophotometer; (2) sb2O3Conversion determination-Sb of antimony pentoxide colloids prepared in examples 1 to 4 was tested using cerium sulfate as a titrant and 0.1% methyl orange as an indicator2O3Conversion rate; (3) particle size test-the antimony pentoxide colloids of examples 1-4 were subjected to a particle size test using a Zetasizer 3000HS laser particle sizer, the test results are shown in table 1,
table 1. test results:
as can be seen from Table 1, the antimony pentoxide colloids prepared in examples 1 to 4 of the present invention have particle sizes of 4.23 to 5.11nm, smaller particle sizes, light transmittance of 97.21% or more, and Sb2O3The conversion rates are all above 94.69%, which shows that the antimony pentoxide colloid of the invention has good physical properties.
Claims (8)
1. The preparation method of the antimony pentoxide colloid for flame retardance of the textile is characterized by comprising the following steps of:
s1: uniformly mixing antimony trioxide powder and peroxide, adding the mixture into a container, dropwise adding distilled water, heating to 90-100 ℃ after dropwise adding, and carrying out condensation reflux stirring for 1-2 hours to obtain antimony pentoxide sol;
s2: heating, evaporating and concentrating the antimony pentoxide sol obtained in the step S1 in a water bath at 95-100 ℃ until the water content is 40-45% to obtain antimony pentoxide powder, dispersing the antimony pentoxide powder in an aqueous solution of sodium dodecyl benzene sulfonate and benzylamine, stirring at room temperature for 2-5 h, and performing suction filtration to obtain modified antimony pentoxide sol;
s3: removing sodium ions or potassium ions in the antimony pentoxide sol in the step S2 at 30-35 ℃ by using cation exchange resin, and keeping the pH value in the sol at 6.5-6.8 after ion exchange;
s4: heating the antimony pentoxide sol obtained in the step S3 at 95-98 ℃, evaporating, concentrating to 46-48%, adding lactic acid into the concentrated sol, stirring for 30-60 min, heating in a water bath at 50-70 ℃, dropwise adding an ethanol solution, and stirring for 1-2 h after dropwise adding to obtain the antimony pentoxide sol.
2. The method for preparing antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein the peroxide is any one of sodium peroxide and potassium peroxide.
3. The method for preparing antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein the mass ratio of the antimony trioxide powder to the peroxide is (1.55-1.75) to (1-1.26).
4. The method for preparing antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein the mass ratio of the antimony trioxide powder to the triethylamine is (1-2) to (0.12-0.24).
5. The preparation method of the antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein the mass-to-volume ratio of the antimony trioxide powder to the distilled water is (1-2) g (25-60) mL.
6. The method for preparing antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein the dropping rate of distilled water in the step S1 is 0.15-0.20 mL/S, and the dropping time is 6-10 min; then dropwise adding the mixture to the required solution amount at the dropwise adding rate of 0.36-0.4 mL/s.
7. The method for preparing antimony pentoxide colloid for flame retardancy of textile fabrics according to claim 1, wherein the cation exchange resin is any one selected from cation exchange resin 001 x 7, cation exchange resin 201 x 7, cation exchange resin D001 and cation exchange resin D113.
8. The method for preparing antimony pentoxide colloid for flame retardance of textile fabrics according to claim 1, wherein in the step S4, the amount of the added lactic acid is 8-15% of the sol in the step S3; the dripping rate of the ethanol is 0.2-35 mL/s, and the dripping time is 400-800 s.
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| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1550453A (en) * | 2003-03-27 | 2004-12-01 | 日产化学工业株式会社 | Antimonic oxide sol and method for its preparation |
| US20080038187A1 (en) * | 2004-09-21 | 2008-02-14 | Nissan Chemical Industries, Ltd. | Process for Producing Antimony Pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
-
2021
- 2021-05-06 CN CN202110490638.8A patent/CN113209914A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1550453A (en) * | 2003-03-27 | 2004-12-01 | 日产化学工业株式会社 | Antimonic oxide sol and method for its preparation |
| US20080038187A1 (en) * | 2004-09-21 | 2008-02-14 | Nissan Chemical Industries, Ltd. | Process for Producing Antimony Pentaoxide |
| CN101798112A (en) * | 2010-03-25 | 2010-08-11 | 中南大学 | Method for preparing antimony pentoxide hydrosol and dry powder thereof by using composite stabilizer |
| CN104828866A (en) * | 2015-06-09 | 2015-08-12 | 锡矿山闪星锑业有限责任公司 | Colloidal antimony oxide powder low in volatility at high temperature and preparing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748231A (en) * | 2020-06-28 | 2020-10-09 | 四川硅迪新材料有限公司 | Synthesis method of antimony oxide sol and flame-retardant auxiliary |
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