CN112048100A - Preparation method of fishing net thread quality enhancer - Google Patents
Preparation method of fishing net thread quality enhancer Download PDFInfo
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- CN112048100A CN112048100A CN202010942246.6A CN202010942246A CN112048100A CN 112048100 A CN112048100 A CN 112048100A CN 202010942246 A CN202010942246 A CN 202010942246A CN 112048100 A CN112048100 A CN 112048100A
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- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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- C08K3/20—Oxides; Hydroxides
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- C08L2203/00—Applications
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Abstract
The invention discloses a preparation method of a fishing net thread quality reinforcing agent, belonging to the technical field of fishing net thread processing and manufacturing, and comprising the following steps: (1) the invention provides a method for preparing a fishing net thread reinforcing agent, which comprises the steps of cleaning treatment (2), irradiation treatment (3), preparation of mixed liquid A, preparation of mixed liquid B, preparation of reinforcing agent (4), and preparation of reinforcing agent (5).
Description
Technical Field
The invention belongs to the technical field of processing and manufacturing of fishing net threads, and particularly relates to a preparation method of a fishing net thread quality enhancer.
Background
Fishing net thread is common basic raw materials in the fishing tackle field, and originally most make by cotton-flax material, along with people to its service property's continuous promotion and the continuous reinforcing of production technique, current fishing net thread is mostly plastics class synthetic fiber, wherein nylon fishing net thread's proportion is great. Although the nylon fishing net thread has larger usage amount and mature production and processing, the performance requirement of the production and processing of the nylon fishing net thread is continuously enhanced along with the continuous improvement of the product requirement of people.
In order to improve the strength, corrosion resistance, temperature resistance and other qualities of the nylon fishing net thread, the existing processes are improved by adding filler components, common fillers comprise kaolin, attapulgite and the like, and although a certain improvement effect is achieved, the use effect of the fillers is limited due to the problems that filler particles are easy to agglomerate, poor in dispersity, poor in compatibility with a high polymer material matrix, single in function and the like.
Therefore, it is necessary to develop a novel filler reinforcing agent which can better improve the comprehensive use characteristics of the fishing net thread.
Disclosure of Invention
The invention aims to provide a preparation method of a fishing net thread quality reinforcing agent aiming at the existing problems.
The invention is realized by the following technical scheme:
a preparation method of a fishing net thread quality reinforcing agent comprises the following steps:
(1) cleaning treatment:
sequentially soaking and cleaning the graphene with acid liquor, alkali liquor and deionized water, and filtering out for later use;
(2) irradiation treatment:
placing the graphene treated in the step (1) into an irradiation box for irradiation treatment, and taking out for later use after the irradiation treatment is completed;
(3) preparing a mixed solution A:
uniformly mixing the graphene treated in the step (2), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water, and then heating for 55-65 min to obtain a mixed solution A for later use;
(4) preparing a mixed solution B:
uniformly mixing the zirconium oxychloride solution and hydrogen peroxide, and stirring at a high speed for 20-25 min to obtain a mixed solution B for later use;
(5) preparing an enhancer:
and (4) adding the mixed solution A obtained in the step (3) into the mixed solution B obtained in the step (4), carrying out ultrasonic treatment for 25-30 min, adjusting the pH value of the whole to 6.8-7.2, and finally carrying out centrifugation and drying treatment to obtain the reinforcing agent.
Further, the acid solution in the step (1) is a phytic acid solution with the mass fraction of 1-1.5%; the alkali liquor is a sodium hydroxide solution with the mass fraction of 1.5-2.0%; the time length of each soaking and cleaning treatment is 15-20 min.
Further, during the irradiation treatment in the step (2), controlling the irradiation box to be subjected to ultraviolet irradiation treatment, wherein the irradiation power is controlled to be 2300-2400W; the irradiation time is 30-40 min.
Further, when the graphene treated in the step (2) in the step (3), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water are mixed together, the corresponding weight ratio is 8-10: 3-5: 2-4: 1-3: 4-7: 2-3: 0.3-0.5: 160-180 parts.
Further, the surfactant is an anionic surfactant; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570; the nano filler is nano zinc oxide or nano titanium nitride.
Further, the temperature of the whole is maintained at 82 to 86 ℃ during the heat treatment in the step (3).
Further, the volume ratio of the zirconium oxychloride solution in the step (4) to the hydrogen peroxide is 2.5-3.5: 1; the concentration of the zirconium oxychloride solution is 0.22-0.25 mol/L; the volume fraction of the hydrogen peroxide is 35-38%; and the rotating speed of stirring is controlled to be 2400-2600 rpm during high-speed stirring treatment.
Further, the ultrasonic frequency is controlled to be 600-700 kHz during ultrasonic treatment in the step (5).
Further, the centrifugal rotating speed in the step (5) is 8000-8500 rpm; and during the drying treatment, the drying temperature is controlled to be 70-75 ℃.
Compared with the prior art, the invention has the following advantages:
the invention provides a method for preparing a fishing net thread reinforcing agent, which has simple integral process, reasonable matching of all steps and easy commercial application and popularization; in the preparation process, firstly, graphene is soaked and cleaned, the surface of the graphene is cleaned, the subsequent processing treatment is facilitated, then, the graphene is irradiated, the surface active group type and activity of the graphene are well improved by ultraviolet irradiation treatment, the reaction capability is enhanced, then, a mixed solution A is prepared by blending the components of the graphene and the like, then, a mixed solution B is prepared by mixing a zirconium oxychloride solution and hydrogen peroxide together, finally, a reinforcing agent is prepared by blending the mixed solution A and the mixed solution B, the graphene in the mixed solution A is subjected to intercalation grafting modification by nano fillers in the graphene, the graphene has larger specific surface area and adsorption capability and higher stability and activity, and during the blending reaction with the mixed solution B, zirconium sol particles in the mixed solution B are adsorbed and fixed on the outer surface layer of graphene matrix particles, so that a stable coating modified layer is obtained, therefore, the service characteristics of the graphene are remarkably improved, the finally prepared reinforcing agent has strong compatible binding force with the fishing net thread substrate component, the use stability is high, the comprehensive use quality of the fishing net thread can be stably improved, and the popularization and application value and the market competitiveness are high.
Detailed Description
Example 1
A preparation method of a fishing net thread quality reinforcing agent comprises the following steps:
(1) cleaning treatment:
sequentially soaking and cleaning the graphene with acid liquor, alkali liquor and deionized water, and filtering out for later use;
(2) irradiation treatment:
placing the graphene treated in the step (1) into an irradiation box for irradiation treatment, and taking out for later use after the irradiation treatment is completed;
(3) preparing a mixed solution A:
uniformly mixing the graphene treated in the step (2), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water, and then heating for 55-65 min to obtain a mixed solution A for later use;
(4) preparing a mixed solution B:
uniformly mixing the zirconium oxychloride solution and hydrogen peroxide, and stirring at a high speed for 20min to obtain a mixed solution B for later use;
(5) preparing an enhancer:
and (4) adding the mixed solution A obtained in the step (3) into the mixed solution B obtained in the step (4), carrying out ultrasonic treatment for 25min, adjusting the pH value of the whole to 6.8, and finally carrying out centrifugation and drying treatment to obtain the reinforcing agent.
The acid solution in the step (1) is a phytic acid solution with the mass fraction of 1%; the alkali liquor is a sodium hydroxide solution with the mass fraction of 1.5%; the time length of each soaking and cleaning treatment is 15 min.
Controlling the irradiation box to be subjected to ultraviolet irradiation treatment during the irradiation treatment in the step (2), wherein the irradiation power is controlled to be 2300W; the irradiation time is 30 min.
When the graphene treated in the step (2) in the step (3), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water are mixed together, the corresponding weight ratio is 8:3:2: 1: 4:2:0.3: 160; the surfactant is an anionic surfactant; the silane coupling agent is a silane coupling agent kh 550; the nano filler is nano zinc oxide; the temperature of the whole was maintained at 82 ℃ during the heat treatment.
The corresponding volume ratio of the zirconium oxychloride solution in the step (4) to the hydrogen peroxide is 2.5: 1; the concentration of the zirconium oxychloride solution is 0.22 mol/L; the volume fraction of the hydrogen peroxide is 35 percent; the rotating speed of stirring is controlled to be 2400rpm during the high-speed stirring treatment.
Controlling the ultrasonic frequency to be 600kHz during the ultrasonic treatment in the step (5); the centrifugal rotating speed during centrifugation is 8000 rpm; the drying temperature is controlled to be 70 ℃ during the drying treatment.
Example 2
A preparation method of a fishing net thread quality reinforcing agent comprises the following steps:
(1) cleaning treatment:
sequentially soaking and cleaning the graphene with acid liquor, alkali liquor and deionized water, and filtering out for later use;
(2) irradiation treatment:
placing the graphene treated in the step (1) into an irradiation box for irradiation treatment, and taking out for later use after the irradiation treatment is completed;
(3) preparing a mixed solution A:
uniformly mixing the graphene treated in the step (2), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water, and then heating for 60min to obtain a mixed solution A for later use;
(4) preparing a mixed solution B:
uniformly mixing the zirconium oxychloride solution and hydrogen peroxide, and stirring at a high speed for 23min to obtain a mixed solution B for later use;
(5) preparing an enhancer:
and (4) adding the mixed solution A obtained in the step (3) into the mixed solution B obtained in the step (4), carrying out ultrasonic treatment for 28min, adjusting the pH value of the whole to 7.0, and finally carrying out centrifugation and drying treatment to obtain the reinforcing agent.
The acid solution in the step (1) is a phytic acid solution with the mass fraction of 1.3%; the alkali liquor is a sodium hydroxide solution with the mass fraction of 1.8%; the time length of each soaking and cleaning treatment is 19 min.
During the irradiation treatment in the step (2), the ultraviolet irradiation treatment is controlled in the irradiation box, and the irradiation power is controlled to be 2350W; the irradiation time was 35 min.
When the graphene treated in the step (2) in the step (3), the surfactant, the polyethylene glycol, the zinc stearate, the silane coupling agent, the nano-filler, the disodium ethylene diamine tetraacetate and the deionized water are mixed together, the corresponding weight ratio is 9:4:3: 2: 6:2.5:0.4: 170; the surfactant is an anionic surfactant; the silane coupling agent is a silane coupling agent kh 560; the nano filler is nano zinc oxide; the temperature of the whole was maintained at 85 ℃ during the heat treatment.
The corresponding volume ratio of the zirconium oxychloride solution in the step (4) to the hydrogen peroxide is 3: 1; the concentration of the zirconium oxychloride solution is 0.24 mol/L; the volume fraction of the hydrogen peroxide is 37 percent; the rotating speed of stirring is controlled to be 2500rpm during the high-speed stirring treatment.
Controlling the ultrasonic frequency to be 670kHz during the ultrasonic treatment in the step (5); the centrifugal rotating speed during centrifugation is 8300 rpm; the drying temperature is controlled to be 72 ℃ during the drying treatment.
Example 3
A preparation method of a fishing net thread quality reinforcing agent comprises the following steps:
(1) cleaning treatment:
sequentially soaking and cleaning the graphene with acid liquor, alkali liquor and deionized water, and filtering out for later use;
(2) irradiation treatment:
placing the graphene treated in the step (1) into an irradiation box for irradiation treatment, and taking out for later use after the irradiation treatment is completed;
(3) preparing a mixed solution A:
uniformly mixing the graphene treated in the step (2), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water, and then heating for 65min to obtain a mixed solution A for later use;
(4) preparing a mixed solution B:
uniformly mixing the zirconium oxychloride solution and hydrogen peroxide, and stirring at a high speed for 25min to obtain a mixed solution B for later use;
(5) preparing an enhancer:
and (4) adding the mixed solution A obtained in the step (3) into the mixed solution B obtained in the step (4), carrying out ultrasonic treatment for 30min, adjusting the pH value of the whole to 7.2, and finally carrying out centrifugation and drying treatment to obtain the reinforcing agent.
The acid solution in the step (1) is a phytic acid solution with the mass fraction of 1.5%; the alkali liquor is a sodium hydroxide solution with the mass fraction of 2.0%; the time length of each soaking and cleaning treatment is 20 min.
Controlling the irradiation box to carry out ultraviolet irradiation treatment during the irradiation treatment in the step (2), wherein the irradiation power is controlled to be 2400W; the irradiation time is 40 min.
When the graphene treated in the step (2) in the step (3), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water are mixed together, the corresponding weight ratio is 10:5:4: 3: 7:3:0.5: 180 of the total weight of the composition; the surfactant is an anionic surfactant; the silane coupling agent is a silane coupling agent kh 570; the nano filler is nano zinc oxide or nano titanium nitride; the temperature of the whole was maintained at 86 ℃ during the heat treatment.
The corresponding volume ratio of the zirconium oxychloride solution in the step (4) to the hydrogen peroxide is 3.5: 1; the concentration of the zirconium oxychloride solution is 0.25 mol/L; the volume fraction of the hydrogen peroxide is 38 percent; the rotating speed of stirring is controlled to be 2600rpm during the high-speed stirring treatment.
Controlling the ultrasonic frequency to be 700kHz during the ultrasonic treatment in the step (5); the centrifugal rotating speed during centrifugation is 8500 rpm; the temperature for controlling the drying is 75 ℃ during the drying treatment.
Comparative example 1
This comparative example 1 is different from example 2 only in that the irradiation treatment operation of step (2) is omitted except that the process steps are the same.
Comparative example 2
In comparison with example 2, comparative example 2 omits the nanofiller component in the preparation of mixture a in step (3), except that the process steps are otherwise the same.
Comparative example 3
Compared with the example 2, the comparative example 3 omits the preparation of the mixed liquid B in the step (4) and the corresponding operation of the subsequent mixed liquid B, except that the steps of the other methods are the same.
Control group
Common graphene components are currently commercially available as reinforcing agents.
In order to compare the effects of the invention, the reinforcing agents prepared by the above example 2, comparative example 1, comparative example 2, comparative example 3 and control group are used in the preparation of nylon fishing net thread, the weight percentage of the reinforcing agents is 5%, after the completion of the preparation, the performance test is carried out on the nylon fishing net thread (the monofilament diameter specification is 0.20 +/-0.01 mm), and the specific comparative data are shown in the following table 1:
TABLE 1
Note: the breaking strength described in table 1 above was measured by a british INSTRON-4466 type force tester, and during the test, the temperature was controlled at 20 ± 2 ℃, the relative humidity was controlled at 65 ± 5%, the drawing speed was controlled at 330mm/min, and the length of the monofilament was 600 mm; the knot strength retention rate is measured after all groups of nylon fishing net threads which are correspondingly treated are exposed for 12 months under natural conditions that the temperature is 35 ℃ and the relative humidity is 85 percent so as to reflect the corrosion-resistant and anti-aging characteristics of the nylon fishing net threads.
As can be seen from the above table 1, the reinforcing agent prepared by the method of the invention can significantly and effectively improve the use strength, corrosion resistance, weather resistance and other qualities of the fishing net thread, significantly improve the service life of the fishing net thread, and has great market competitiveness and economic benefits.
Claims (9)
1. A preparation method of a fishing net thread quality reinforcing agent is characterized by comprising the following steps:
(1) cleaning treatment:
sequentially soaking and cleaning the graphene with acid liquor, alkali liquor and deionized water, and filtering out for later use;
(2) irradiation treatment:
placing the graphene treated in the step (1) into an irradiation box for irradiation treatment, and taking out for later use after the irradiation treatment is completed;
(3) preparing a mixed solution A:
uniformly mixing the graphene treated in the step (2), a surfactant, polyethylene glycol, zinc stearate, a silane coupling agent, a nano filler, disodium ethylene diamine tetraacetate and deionized water, and then heating for 55-65 min to obtain a mixed solution A for later use;
(4) preparing a mixed solution B:
uniformly mixing the zirconium oxychloride solution and hydrogen peroxide, and stirring at a high speed for 20-25 min to obtain a mixed solution B for later use;
(5) preparing an enhancer:
and (4) adding the mixed solution A obtained in the step (3) into the mixed solution B obtained in the step (4), carrying out ultrasonic treatment for 25-30 min, adjusting the pH value of the whole to 6.8-7.2, and finally carrying out centrifugation and drying treatment to obtain the reinforcing agent.
2. The method for preparing the fishing net thread quality enhancer according to claim 1, wherein the acid solution in the step (1) is a phytic acid solution with a mass fraction of 1-1.5%; the alkali liquor is a sodium hydroxide solution with the mass fraction of 1.5-2.0%; the time length of each soaking and cleaning treatment is 15-20 min.
3. The method for preparing the fishing net thread quality enhancer according to claim 1, wherein during the irradiation treatment in the step (2), the irradiation box is controlled to be ultraviolet irradiation treatment, and the irradiation power is controlled to be 2300-2400W; the irradiation time is 30-40 min.
4. The preparation method of the fishing net thread quality enhancer according to claim 1, wherein the weight ratio of the graphene treated in the step (2) in the step (3) to the surfactant to the polyethylene glycol to the zinc stearate to the silane coupling agent to the nanofiller to the disodium edetate to the deionized water is 8-10: 3-5: 2-4: 1-3: 4-7: 2-3: 0.3-0.5: 160-180 parts.
5. The method for preparing the fishing net thread quality enhancer according to claim 4, wherein the surfactant is an anionic surfactant; the silane coupling agent is any one of a silane coupling agent kh550, a silane coupling agent kh560 and a silane coupling agent kh 570; the nano filler is nano zinc oxide or nano titanium nitride.
6. The method for preparing a reinforcing agent for the quality of fishing net threads according to claim 1, wherein the temperature of the whole is maintained at 82 to 86 ℃ during the heating treatment in the step (3).
7. The preparation method of the fishing net thread quality enhancer according to claim 1, wherein the corresponding volume ratio of the zirconium oxychloride solution and the hydrogen peroxide in the step (4) is 2.5-3.5: 1; the concentration of the zirconium oxychloride solution is 0.22-0.25 mol/L; the volume fraction of the hydrogen peroxide is 35-38%; and the rotating speed of stirring is controlled to be 2400-2600 rpm during high-speed stirring treatment.
8. The method for preparing the reinforcing agent for the quality of the fishing net thread according to claim 1, wherein the ultrasonic frequency is controlled to be 600-700 kHz during the ultrasonic treatment in the step (5).
9. The method for preparing the reinforcing agent for the quality of the fishing net thread according to claim 1, wherein the centrifugal rotation speed in the centrifugation in the step (5) is 8000-8500 rpm; and during the drying treatment, the drying temperature is controlled to be 70-75 ℃.
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2020
- 2020-09-09 CN CN202010942246.6A patent/CN112048100A/en not_active Withdrawn
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|---|---|---|---|---|
| GB873171A (en) * | 1944-11-03 | 1961-07-19 | Atomic Energy Authority Uk | Production of u |
| CN106000297A (en) * | 2016-05-10 | 2016-10-12 | 郑州大学 | Graphene loaded zirconium oxide composite material, preparing method thereof, and application thereof as desulfurizer adsorbent |
| CN106832631A (en) * | 2016-12-16 | 2017-06-13 | 江海涛 | A kind of polystyrene construction material of silane-modified carrying transition metal and preparation method thereof |
| CN106824066A (en) * | 2016-12-30 | 2017-06-13 | 贵州科学院 | Modified zirconium hydroxide composite adsorbing material of the 3D Graphenes of fluorine ion and preparation method thereof in a kind of removal rural potable water |
| CN108727876A (en) * | 2018-05-19 | 2018-11-02 | 巢湖市翔宇渔具有限公司 | A kind of preparation method for the filler promoting fishing lines intensity and rotproofness |
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