CN113149448B - Preparation method of direct twistless roving - Google Patents
Preparation method of direct twistless roving Download PDFInfo
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- CN113149448B CN113149448B CN202110459140.5A CN202110459140A CN113149448B CN 113149448 B CN113149448 B CN 113149448B CN 202110459140 A CN202110459140 A CN 202110459140A CN 113149448 B CN113149448 B CN 113149448B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/32—Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C03C25/323—Polyesters, e.g. alkyd resins
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/32—Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C03C25/36—Epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/095—Glass compositions containing silica with 40% to 90% silica, by weight containing rare earths
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a method for preparing direct twistless roving, and belongs to the technical field of inorganic non-metallic materials. The preparation method of the direct twistless roving comprises the following steps: weighing raw materials in proportion, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment, then carrying out spinning forming to obtain glass fibers, coating a sizing agent after cooling, then winding the glass fibers into direct twistless roving by a direct twistless roving drawing machine, and drying the direct twistless roving. According to the invention, through the limitation of the glass fiber raw material and the limitation of the components of the coated sizing agent, the direct twistless roving with high breaking strength, high bending strength of the pultruded bar and small hairiness is successfully obtained.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to a preparation method of direct twistless roving.
Background
Glass fiber (Fiberglass) is an inorganic non-metallic material with excellent performance, has good insulativity, strong heat resistance, good corrosion resistance and high mechanical strength, but is brittle and has poor wear resistance. The hair-care fiber is prepared from six kinds of ores of pyrophyllite, quartz sand, limestone, dolomite, borocalcite and boromagnesite by the processes of high-temperature melting, wire drawing, winding, weaving and the like, wherein the diameter of each monofilament ranges from several micrometers to twenty micrometers, the monofilament is equivalent to 1/20-1/5 of one hair, and each fiber protofilament bundle consists of hundreds of monofilaments or even thousands of monofilaments. Glass fiber is generally used as a reinforcing material, an electrical insulating material, a heat insulating material, a circuit substrate and other inorganic fiber reinforcing materials in composite materials in various fields of national economy, and is the largest inorganic fiber reinforcing material used at present.
The glass fiber direct roving is widely applied to the fields of shipbuilding, wind power blades, petrochemical industry, architectural decoration, heat preservation, heat insulation and the like. Conventional glass fibers are often brittle without surface treatment, and the surface of the glass fibers is often coated with a sizing agent to improve the performance of the glass fibers. The properties of the glass fibers and the special sizing agent are the main influencing factors for improving the properties of the prepared direct roving.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of direct twistless roving; the invention utilizes the specific glass fiber composition, has higher elastic modulus and tensile bending strength on the basis of ensuring better stability, and obtains the direct untwisted roving with less hairiness after being treated by using the special impregnating compound.
In order to solve the technical problems, the invention provides the following technical scheme:
in one aspect, the present invention provides a method of making a direct twistless roving, comprising: weighing raw materials in proportion, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment, then carrying out spinning forming to obtain glass fibers, coating a sizing agent after cooling, then winding the glass fibers into direct twistless roving by a direct twistless roving drawing machine, and drying the direct twistless roving; wherein:
the impregnating compound consists of the following components in parts by weight: 1-5 parts of aminosilane coupling agent, 10-20 parts of water-soluble epoxy resin, 10-20 parts of polyurethane resin emulsion, 1-5 parts of dodecyl trimethyl ammonium chloride, 1-5 parts of polyoxyethylene ether glycidyl sorbitol, 1-3 parts of pH regulator and 40-60 parts of deionized water.
Further, the raw materials comprise the following components in percentage by weight:
preferably, the raw materials consist of the following components in percentage by weight:
further, said R 2 O is Na 2 O、K 2 O and Li 2 A mixture of O; wherein Li 2 O stands for R 2 50-60% of the total weight of O.
Further, caO and Al are mentioned 2 O 3 And MgO in a weight ratio of 1; ce 2 O 3 /Yb 2 O 3 The weight ratio of (A) to (B) is 1.
Preferably, the CaO and Al are 2 O 3 And MgO in a weight ratio of 1; ce 2 O 3 /Yb 2 O 3 The weight ratio is 1.
Preferably, the pH adjusting agent is citric acid.
Preferably, the melting temperature is 1300-1400 ℃.
Preferably, the spinning temperature is 1200 to 1300 ℃.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the invention greatly optimizes the glass fiber raw materials, so that the raw materials have synergistic effect, and the prepared direct twistless roving has higher bending breaking strength.
SiO in the invention 2 The skeleton main body for forming glass is a network forming object, and in order to improve the modulus of glass fiber, the invention reduces SiO to a certain extent 2 In order to ensure chemical stability and mechanical strength, siO is limited 2 The content is 54-57%.
Al 2 O 3 The addition of (2) has an influence on the crystallization tendency, stability and mechanical strength of the glass fiber, and the stability and mechanical strength of the glass fiber can be improved when the addition amount is higher, but the crystallization rate is increased, the melting difficulty is improved, the viscosity is increased, and the difficulty in the glass melting process is increased. In order to adjust the viscosity of the glass and the crystallization of the glass, certain content of CaO and MgO is added, and CaO and Al are subjected to crystallization 2 O 3 The weight ratio of (a) to (b), reducing the viscosity of the glass; meanwhile, the crystallization tendency can be effectively reduced and the strength can be improved to a certain extent by adjusting the proportion of the dosage of CaO and MgO. Further, ce 2 O 3 、Yb 2 O 3 、ZrO 2 BaO and the like are good fluxes, and can reduce the difficulty in melting to some extent.
The invention is on SiO 2 And Al 2 O 3 The network is formed by introducing calcium, magnesium, cerium, ytterbium, zirconium, barium and the like, and by limiting the addition amount of each substance, particularly CaO/Al 2 O 3 MgO and Ce 2 O 3 /Yb 2 O 3 The weight ratio of (2) is that the network is tighter by utilizing the synergistic effect among all the ions, and all the ions are difficult to move in the network, so that the elastic modulus is improved, and meanwhile, the prepared direct twistless roving has higher breaking strength.
Meanwhile, the impregnating compound is prepared from the aminosilane coupling agent, the polyurethane resin emulsion, the water-soluble epoxy resin, the dodecyl trimethyl ammonium chloride and the polyoxyethylene ether glycidyl sorbitol, so that the breaking strength of the prepared direct twistless roving can be improved, a raw material guarantee is provided for a glass fiber textile product with high requirements, the performance of the glass fiber direct twistless roving can be improved, the hairiness generated by weaving is less, the breaking strength of the direct twistless roving is higher, and the production performance and the application performance are better.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
In the present invention, the materials and reagents used are not specifically described, and are commercially available.
The invention provides a preparation method of direct twistless roving, and specific examples are as follows.
Example 1
A method of making a direct twistless roving, comprising the steps of: weighing raw materials according to the formula of example 1 in the table 1, putting the raw materials into a glass melting furnace, carrying out vitrification and 1300-1400 ℃ melting treatment, and then carrying out spinning forming at 1200-1300 ℃ to obtain the glass fiber. After cooling, coating the impregnating compound, then winding the direct roving into direct twistless roving by a direct twistless roving drawing machine, and drying the direct twistless roving at 110 ℃; wherein: the amount of the impregnating compound is 0.1 percent of the weight of the glass fiber; and the amounts of the components of the impregnating compound are shown in example 1 in Table 2. And the prepared direct twistless roving was subjected to performance testing, the results of which are shown in table 3.
Examples 2 to 8
The raw materials are weighed according to the formulas of the examples 2 to 8 in the table 1, the dosage of each component of the impregnating compound is respectively shown in the examples 2 to 8 in the table 2, and the rest conditions are the same as the example 1.
To further illustrate the beneficial effects of the present invention, a comparative example was constructed as follows, using example 3 as an example only, for reasons of space.
Comparative example 1
Yb of 2 O 3 Is replaced by equal amountLa of 2 O 3 The remaining conditions were the same as in example 3.
Comparative example 2
Yb of 2 O 3 Is replaced by equal amount of Y 2 O 3 The other conditions were the same as in example 3.
Comparative examples 3 to 7
The raw materials were weighed in accordance with the formulations of comparative examples 3 to 7 in Table 1, and the other conditions were the same as in example 1.
Comparative example 8
The aminosilane coupling agent was replaced with the same amount of the vinylsilane coupling agent, and the other conditions were the same as in example 3.
Comparative example 9
The same procedure as in example 3 was repeated except that polyoxyethylene ether sorbitan was replaced with an equivalent amount of fatty alcohol-polyoxyethylene ether.
Comparative example 10
The dosage of the raw materials of the invention is replaced by each raw material formula of the embodiment 5 in the patent CN103396001A, and the rest conditions are the same as the embodiment 3.
2400Tex direct untwisted rovings were produced in the inventive examples and comparative examples, the amount of hairiness produced by a certain amount of direct untwisted rovings during the manufacturing process was determined, and the breaking strength was tested according to GB/T7690.3-2001. And the direct untwisted roving prepared in the examples and the comparative examples is used for reinforcing the performance test of the unsaturated polyester resin pultrusion bar with the diameter of 6 mm.
The direct untwisted rovings prepared in examples 1-8 were tested for properties and the results are shown in Table 3. The direct untwisted rovings prepared in comparative examples 1 to 10 were tested for properties and the results are shown in table 4.
TABLE 1
TABLE 2
TABLE 3
| Serial number | Amount of feather is mg/kg | Breaking strength N/Tex | The bending strength of the pultruded bar is MPa |
| Example 1 | 1.12 | 62.3 | 1246 |
| Example 2 | 0.86 | 65.4 | 1285 |
| Example 3 | 0.34 | 72.5 | 1376 |
| Example 4 | 0.52 | 68.7 | 1312 |
| Example 5 | 0.46 | 66.5 | 1325 |
| Example 6 | 0.55 | 70.5 | 1314 |
| Example 7 | 0.89 | 68.7 | 1283 |
| Example 8 | 0.42 | 71.2 | 1354 |
As can be seen from tables 1 to 3, the present invention is based on SiO 2 、Al 2 O 3 、Ce 2 O 3 、Yb 2 O 3 、ZrO 2 The BaO and the like, and selects specific impregnating compound components, so that the prepared direct twistless roving has higher breaking strength and bending strength of a pultrusion bar, and meanwhile, the hairiness amount is less in the spinning process.
TABLE 4
As can be seen from tables 1 to 4, yb in the present invention was compared with comparative examples 1 to 3 2 O 3 Respectively replaced by La 2 O 3 Or Y 2 O 3 、Ce 2 O 3 The resulting composition had a relatively low breaking strength and a relatively low flexural strength of the pultruded rods as compared to the examples. This is probably because the difference between the ionic radii of Yb ions and La, Y and Ce ions is large, and Yb can enter SiO well 2 And Al 2 O 3 The formed network prevents ions from moving in the network, so that the network has higher elastic modulus and stability, and the prepared direct untwisted roving has higher strength due to higher elastic modulus to a certain extent.
As can be seen from the data in Table 3, the direct twistless rovings obtained in different ratio ranges have larger difference between the breaking strength and the bending strength of the pultruded rods than the comparative examples 4 to 7, while the CaO/Al in the specific ratio range of the present invention 2 O 3 MgO and Ce 2 O 3 /Yb 2 O 3 In a weight ratio of (A) and R 2 Li in O 2 And the dosage proportion of O can obtain the direct twistless roving with the breaking strength and the bending strength of the pultruded bar.
Compared with the comparative examples 8-9, after the specific components in the impregnating compound are replaced, the breaking strength of the direct roving, the bending strength of the pultrusion bar and the like are greatly influenced, and meanwhile, the hairiness difference in the spinning process is also large. The specific impregnating compound has good permeability, so that a good coating film can be formed on the surface of the glass fiber, and hairiness of the glass fiber is prevented from being generated in the spinning process. Compared with the comparative example 10, the raw materials of the glass fiber are different, which has larger influence on the performance of the prepared direct twistless roving in all aspects, the raw material formula of the invention is reasonable, and the prepared direct twistless roving has higher strength.
In conclusion, the invention successfully obtains the direct twistless roving with high breaking strength and bending strength of the pultruded bar and less hairiness by limiting the glass fiber raw material and the components of the coated sizing agent.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and are intended to be within the scope of the invention.
Claims (6)
1. A method of making a direct twistless roving, comprising: weighing raw materials in proportion, putting the raw materials into a glass melting furnace, carrying out vitrification and melting treatment, then carrying out spinning forming to obtain glass fibers, coating a sizing agent after cooling, then winding the glass fibers into direct twistless roving by a direct twistless roving drawing machine, and drying the direct twistless roving; wherein:
the impregnating compound comprises the following components in parts by weight: 1-5 parts of aminosilane coupling agent, 10-20 parts of water-soluble epoxy resin, 10-20 parts of polyurethane resin emulsion, 1-5 parts of dodecyl trimethyl ammonium chloride, 1-5 parts of polyoxyethylene ether glycidyl sorbitol, 1-3 parts of pH regulator and 40-60 parts of deionized water; the raw materials consist of the following components in percentage by weight:
SiO 2 54-57wt％；
Al 2 O 3 14-18wt％；
CaO 12-18wt％；
MgO 5-10.5wt％；
Ce 2 O 3 1-5wt％；
Yb 2 O 3 0.5-3.5wt％；
ZrO 2 0.2-0.5wt％；
BaO 0.1-0.5wt％；
R 2 O 0.7-1.0wt％；
CaO and Al 2 O 3 And MgO in a weight ratio of 1, 0.88-1.5; ce 2 O 3 /Yb 2 O 3 The weight ratio of (1);
the R is 2 O is Na 2 O、K 2 O and Li 2 A mixture of O; wherein Li 2 O stands for R 2 50-60% of the total weight of O.
2. The method of making a direct twistless roving of claim 1, wherein said starting material consists of the following components in weight percent:
SiO 2 55-56wt％；
Al 2 O 3 15-18wt％；
CaO 14-16wt％；
MgO 6-8wt％；
Ce 2 O 3 2-5wt％；
Yb 2 O 3 1-3.5wt％；
ZrO 2 0.2-0.5wt％；
BaO 0.3-0.5wt％；
R 2 O 0.8-0.9wt％。
3. method for making direct twistless rovings according to claim 2, wherein the CaO, al 2 O 3 And MgO in a weight ratio of 1-1.5; ce 2 O 3 /Yb 2 O 3 The weight ratio is 1.
4. The method of making a direct twistless roving of claim 3, wherein said pH adjusting agent is citric acid.
5. The method of making a direct twistless roving of claim 1, wherein said melting temperature is from 1300 ℃ to 1400 ℃.
6. Method for making direct twistless rovings according to claim 1, wherein the spinning temperature is 1200-1300 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100356A (en) * | 2007-06-12 | 2008-01-09 | 巨石集团有限公司 | Direct untwisted roving soaking agent |
| CN110818284A (en) * | 2019-12-16 | 2020-02-21 | 巨石集团有限公司 | Glass fiber strand twistless roving impregnating compound, preparation method, product and application |
| CN112374769A (en) * | 2020-04-20 | 2021-02-19 | 河南光远新材料股份有限公司 | Impregnating compound for glass fiber spun yarn and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7795354B2 (en) * | 2006-06-16 | 2010-09-14 | Georgia-Pacific Chemicals Llc | Formaldehyde free binder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101100356A (en) * | 2007-06-12 | 2008-01-09 | 巨石集团有限公司 | Direct untwisted roving soaking agent |
| CN110818284A (en) * | 2019-12-16 | 2020-02-21 | 巨石集团有限公司 | Glass fiber strand twistless roving impregnating compound, preparation method, product and application |
| CN112374769A (en) * | 2020-04-20 | 2021-02-19 | 河南光远新材料股份有限公司 | Impregnating compound for glass fiber spun yarn and preparation method thereof |
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