# US 11,306,200 B2 · Method for preparing organometallic composite material

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- Number: US 11,306,200 B2
- Document ID: US11306200B2
- Status: Granted
- Kind: B2
- Application number: 16/858,739
- Filed: 2020-04-27
- Published: 2020-12-31
- Granted: 2022-04-19
- Earliest claimed: 2019-06-27
- Assignees: Changzhou University
- Applicants: Changzhou University
- Inventors: Qun Chen; Haiqun Chen; Jian Lu; Chunping Fang; Wen Yi; Feng Li; Shuhua Wang; Zhongjing Chen; Lina Zhang; Mingyang He
- Web page: https://patentgrep.com/patent/US11306200B2

## CPC

- B29C 48/16: Articles comprising two or more components, e.g. co-extruded layers
- C08L 27/06: Homopolymers or copolymers of vinyl chloride
- B29C 48/022: {characterised by the choice of material}
- B29C 48/13: Articles with a cross-section varying in the longitudinal direction, e.g. corrugated pipes
- B29C 48/40: using two or more parallel screws {or at least two parallel non-intermeshing screws}, e.g. twin screw extruders
- B29C 48/911: {Cooling}
- B29C 48/92: Measuring, controlling or regulating
- C08K 3/041: {Carbon nanotubes}
- C08K 3/22: of metals
- C08K 3/26: Carbonates; Bicarbonates
- C08K 3/30: Sulfur-, selenium- or tellurium-containing compounds
- C08K 5/098: Metal salts of carboxylic acids
- C08K 7/02: Fibres or whiskers
- B29C 2948/9259: Angular velocity
- B29C 2948/92704: Temperature
- B29K 2027/06: PVC, i.e. polyvinylchloride
- C08K 2003/2241: {Titanium dioxide}
- C08K 2003/262: {Alkali metal carbonates}
- C08K 2003/265: {Calcium, strontium or barium carbonate}
- C08K 2003/3045: {Sulfates}
- C08K 2201/005: Additives being defined by their particle size in general
- C08L 2205/03: containing three or more polymers in a blend
- C08L 2205/16: Fibres; Fibrils
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS

## Abstract

The present invention provides a method for preparing organometallic composite material, comprising: providing PVC resin, activated calcium carbonate, plant fiber, calcium stearate, barium sulfate, paraffin, sodium bicarbonate, zinc laurate, nanometre titanium dioxide, organometallic salt, shell powder, carbon nanotube, talcum powder and stabilizer; mixing and heating; subject to first cooling after extrusion and second cooling under vacuum; towing to obtain the organometallic composite material, wherein the organometallic salt is a benzoic acid metal salt mixture. The present method can significantly reduce the processing temperature of PVC composite by 20 to 50° C., and also increase the toughness and strength of the material so as to alleviate the exudation of the composite material as in the conventional technologies and extend the lifespan of the composite material.

## Claims

### Claim 1

A method for preparing a composite material, comprising:
providing a PVC resin, an activated calcium carbonate, a plant fiber, calcium stearate, barium sulfate, paraffin wax, sodium bicarbonate, zinc laurate, nanometer-sized titanium dioxide, an organometallic salt, shell powder, carbon nanotubes, talcum powder, and a stabilizer to create a first mixture;
mixing and heating the first mixture to obtain a second mixture;
extruding the second mixture to obtain a molded article;
subjecting the molded article to a first cooling to obtain a cooled molded article;
subjecting the cooled molded article to a second cooling under vacuum to obtain the composite material.

### Claim 2 (depends on 1)

The method of claim 1, wherein the organometallic salt is a benzoic acid metal salt represented by the following formula:
wherein n=1, 2 or 3; M is selected from copper, iron, zinc, magnesium, calcium, or combinations thereof.

### Claim 3 (depends on 1)

The method of claim 1, wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass; the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotubes are from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.

### Claim 4 (depends on 2)

The method of claim 2, wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass, the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotubes are from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.

### Claim 5 (depends on 1)

The method of claim 1, wherein the mixing and heating comprises mixing at a first speed from 400 to 500 r/min for 1 to 2 hours at a first temperature from 100 to 120° C., followed by mixing at a second speed from 80 to 120 r/min for 30 to 50 minutes at a second temperature from 30 to 40° C., and wherein said extruding is performed at different temperatures according to different zones: 110 to 120° C. in zone 1; 125 to 135° C. in zone 2; 140 to 150° C. in zone 3; 165 to 175° C. in zone 4; and 105 to 110° C. in a confluence core, and wherein said first cooling is water cooling, and wherein said second cooling under vacuum has a temperature from −10 to −15° C.

### Claim 6 (depends on 1)

The method of claim 1, wherein the mixing and heating comprises mixing at a speed of 450 r/min for 1.1 hours at a temperature of 101° C., followed by mixing at a speed of 80 r/min for 40 minutes at a temperature of 31° C.

### Claim 7 (depends on 1)

A composite material prepared by the method according to claim 1,
wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass; the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotube is from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.

### Claim 8 (depends on 7)

The composite material according to claim 7, wherein the organometallic salt is a benzoic acid metal salt represented by the following formula:
wherein n=1, 2 or 3; M is selected from copper, iron, zinc, magnesium, calcium, or combinations thereof.

### Claim 9 (depends on 7)

The composite material according to claim 7, wherein the material has an exudation rate from 0.3% to 15%.

### Claim 10 (depends on 8)

The composite material according to claim 8, wherein the material has an exudation rate from 0.3% to 15%.