CN111607281A - Metal soft substance and preparation method and application thereof - Google Patents
Metal soft substance and preparation method and application thereof Download PDFInfo
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a metal soft substance and a preparation method and application thereof. The metal soft substance is prepared from the following components: titanium powder with metal content more than 99.5%, a crushing agent and a disintegrating aid, a dispersing agent, a soft substance carrier, a flocculating agent, a precipitation preventing agent and a precipitation preventing agent. The titanium metal soft substance can be added into the epoxy resin, so that the glass transition temperature of the epoxy resin can be increased from 80 ℃ to more than 200 ℃, and no substance which can remarkably increase the glass transition temperature of the epoxy resin is found so far; the titanium-based metal soft substance is added into the epoxy resin coating to endow the coating with anti-scaling performance; the titanium metal soft substance can also obviously improve the temperature resistance and the corrosion resistance of the coating.
Description
Technical Field
The invention relates to the technical field of soft substances, in particular to a metal soft substance and a preparation method and application thereof.
Background
Soft matter is an emerging discipline emerging in recent years, referred to as "complex fluids" in the united states. In 1991, the concept of soft substances is proposed by the Nobel physics awarding hot nals taking the soft substances as the subjects of awarding speeches. Soft materials refer to materials intermediate between solids and desirable fluids, generally consisting of macromolecules or groups, such as liquid crystals, polymers, colloids, films, foams, particulate materials, life system materials, and the like, which are ubiquitous in nature, life, everyday life, and production. Many research institutions all carry out the research on soft substances vigorously internationally, and the soft substances are already in foreign physical textbooks and are not seen at home.
The hard matter is converted into soft matter by a new technology, and the soft matter has qualitative change in property, so that the hard matter has many properties which the original hard matter does not have at all.
Soft matter has two essential features:
1. very weak external action with very strong response
2. Very small amounts of additives can dramatically change the properties of soft material systems.
Soft materials are said to be "soft" compared to hard materials such as metals, semiconductors, ceramics, etc., because there is no hard structure like a solid. It can make relatively obvious response and change to relatively weak external influence, such as small change of material composition or structure, for example transient or weak stimulus applied on the material, etc., i.e. it has the characteristic of weak influence and strong response.
Roughly speaking, soft matter mainly includes two aspects: complexity, variability.
The changeability of the soft substance means that the resistance of the soft substance is weak, the change is usually nonlinear, but the direction and the magnitude of the change of the system can be known.
Hard substance: large stress producing small deformation
Soft matter: small stress producing large deformation
The physicist has been prepared with rubber as an example to illustrate the unusual properties of soft materials. Natural rubber is susceptible to oxidation and breakage in air, but becomes a strong and durable material after vulcanization. The sodium indicates that only 1 atom of every 200 carbon atoms of natural rubber reacts with sulfur. Although the chemical action is so weak, it is sufficient to cause a large change in the physical properties of the rubber from liquid to solid, and the change of the gum into rubber proves that some substances change state due to the weak action, which is the unusual characteristic of soft substances-the weak force causes a strong change.
Where soft materials provide only a relatively weak force, they can undergo a significant change-from shape to property. People can easily understand why one button cell can drive the liquid crystal watch to work for several years; a few drops of liquid detergent will produce a large pile of foam … …. A smell sensitive dog can trace a person according to residual smell in a footprint and distinguish the person's trace from other people in a downtown. Biological systems exhibit the nature of soft matter.
Since the state of the soft matter is between that of a liquid and an ideal solid, molecules in a simple liquid can flow freely, limited only by the container; molecules in an ideal solid move thermally near a fixed position and cannot change sequence, while soft materials have both the thermal fluctuation behavior of liquids and the strong binding self-organization properties of solids.
The inventor of the present invention has carried out a series of studies on a preparation method, a preparation apparatus, an application, and the like of a metal soft substance. The applied patents are granted, such as a CN00209258.1 titanium-based nano metal powder grinding device, a CN00105672.7 titanium-based nano metal powder manufacturing method, CN00132108.0 titanium nano polymer paint and CN03153420.1 a novel titanium nano polymer anticorrosion and antiscale water injection oil pipe.
Disclosure of Invention
The present invention is directed to the solution of the problems found in the above studies and further improvements in performance. Compared with a mixture system formed by mixing metal titanium powder, a grinding aid, a protective agent and a dispersing agent in a certain proportion in the CN00105672.7 titanium-based nano metal powder manufacturing method, the colloidal titanium-based metal soft substance is prepared by a two-step method, and meanwhile, the addition of the grinding aid, the dispersing agent, a soft substance carrier, a flocculating agent and a precipitation preventing agent is found to not only influence the stability of the obtained colloidal titanium-based metal soft substance, but also obtain an unexpected effect on the performance of resin modification. The present invention is based on this finding.
The first aspect of the invention provides a metal soft substance, which is prepared from the following components:
titanium powder with metal content more than 99.5%, a crushing agent and a disintegrating aid, a dispersing agent, a soft substance carrier, an anti-flocculating agent, an anti-precipitation agent and an anti-precipitation agent;
preferably, the composition by weight is:
a crushing agent and a crushing aid which account for 5-10% of the titanium powder;
a dispersant accounting for 0.5-3% of the titanium powder;
soft matter carrier accounting for 100-500% of the titanium powder;
anti-flocculating agent accounting for 0.02-0.2% of the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft matter carrier;
0.02-0.1% of a precipitation preventing agent accounting for the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft substance carrier;
and
and the anti-settling agent accounts for 0.2-1% of the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft matter carrier.
In the invention, the added crushing agent, the auxiliary crushing agent, the dispersing agent and the soft matter carrier are used for assisting the mixing and grinding of titanium powder to obtain the titanium-based soft matter initial polymer with proper particle size distribution. The added anti-flocculant and anti-precipitation agent not only influence the stability of the obtained colloidal titanium-based metal soft substance, but also influence the performance of the resin modification by the colloidal titanium-based metal soft substance.
In some embodiments, the titanium powder is selected from one or more of titanium sponge powder, titanium hydride powder, and alloyed titanium powder.
The requirement for titanium powder also includes that the metal content is more than 99.5 percent. When the content of titanium metal in the titanium powder is less than 99.5%, the performance of the prepared metal soft substance for modifying resin is obviously reduced.
In some embodiments, the size reducing agent is selected from one or more of an epoxy resin and a sulfur-containing rubber.
The crushing agent can significantly affect the crushing effect, namely the particle size, of the titanium powder, and also affect the viscosity and the fluidity of the obtained colloidal titanium-based metal soft substance. It has been found that epoxy resins are superior to sulfur-containing rubbers as a grinding agent.
In some embodiments, the co-comminuting agent is selected from one or more of a silicon coupling agent and a titanate coupling agent.
The pulverizing aid also affects the pulverizing effect, i.e., particle size, of the titanium powder.
In some embodiments, the dispersant is selected from one or more of A-10, HT-5168, HT-5083.
The dispersant may affect the stability of the resulting colloidal titanium-based metal soft material. In the research, it is found that the ground titanium powder obtained by different grinding agents and grinding aids needs different dispersants when in dispersion. For example, HT-5168 is more suitable for the combination of a crushing agent and a co-crushing agent of epoxy resin and a silicon coupling agent than HT-5083, and the obtained colloidal titanium-based metal soft substance has obviously improved glass transition temperature modification on the epoxy resin.
In some embodiments, the soft material carrier used is selected from one or more of a solvent, a reactive diluent, and a polymeric crosslinker.
In some embodiments, the deflocculant is selected from one or more of polyacrylamide, oily amine sulfonate.
In some embodiments, the anti-kogation agent is selected from one or more of oleic acid, stearic acid.
In some embodiments, the anti-settling agent is selected from one or more of R972, BYK 410.
In the research, when the weight ratio of oily amine sulfonate, stearic acid and BYK410 is 1:1 (3-5), the temperature resistance and corrosion resistance of the obtained colloidal titanium-based metal soft substance modified resin are remarkably improved, and the anti-scaling performance is not greatly changed.
A second aspect of the present invention provides a method for producing a metal soft substance according to the first aspect, comprising the steps of:
s01, mixing titanium powder with a crushing agent, a grinding aid, a dispersing agent and a soft matter carrier, and grinding to obtain a titanium-based soft matter primary polymer;
s02, mixing the soft substance primary polymer with a flocculant, a precipitation preventing agent and a precipitation preventing agent, and carrying out colloid treatment to obtain a colloid type titanium-based metal soft substance;
preferably, the milling is carried out in a pulverizer, preferably a high energy planetary pulverizer;
preferably, the peptization treatment is carried out in a ball mill.
The preparation method of the invention comprises two steps: the first step is to utilize a high-energy planetary crusher to carry out metal nanocrystallization processing, and the second step is to realize softening treatment on the nano metal, so that a metal soft substance with special function is obtained and is used for directly modifying resin.
In some embodiments, before the step S01, the method further includes determining the addition amount of the pulverization assisting agent through a test;
the auxiliary crushing agent can be used for accelerating crushing of reaction substances and increasing the contact area of the reaction, wherein the auxiliary crushing agent can increase or decrease the addition amount according to the reaction speed in a test;
firstly, adding a certain amount of pulverization aid with a preset dosage into an equivalent reactant for testing, and obtaining the test heat change according to the following formula;
wherein mu is the variation of test heat quantity, c is the specific heat capacity of the titanium powder, t is the test time, M is the quantity of the added titanium powder, M is the residual quantity of the titanium powder after the test time t, and RwChange in heat to form the said titanium-based soft matter precursor, VsIs the container volume for mixing the titanium powder, the crushing agent, the grinding aid, the dispersing agent and the soft matter carrier,
(ii) a change in heat upon release of the soft material for said soft material carrier f: (i) Is the grinding agent,The heat release function of the pulverization assisting agent and the dispersing agent,1the amount of the grinding agent is expressed,2the amount of the pulverization aid is expressed,3represents the portion of the dispersant;
then, judging the speed of the reaction according to the test heat;
when the test heat is equal to or larger than a preset value, outputting a prompt for reducing the usage amount of the grinding aid agent on the basis of the preset usage amount to preset electronic equipment;
and when the test heat is smaller than a preset value, outputting a prompt of increasing the usage amount of the grinding aid agent on the basis of the preset usage amount to preset electronic equipment.
According to the technical scheme, when the grinding aid is added, whether the quantity of the grinding aid to be added is appropriate is judged through a test, and then the quantity of the grinding aid in subsequent operation is increased or decreased according to the heat change of the test. Therefore, the phenomenon that reaction yield is too slow and time and labor are wasted can be avoided, the phenomenon that resources are wasted due to too fast reaction can be effectively avoided, and the heat change when all reactants are consumed and the heat change when the products are generated are considered in the experimental reaction rate calculation process, so that the calculation result has confidence.
A third aspect of the present invention is to provide a resin comprising the metal soft substance according to the first aspect.
A fourth aspect of the present invention is to provide a use of the metal soft substance according to the first aspect for improving resin properties;
preferably, the resin is an epoxy resin;
preferably, the properties include glass transition temperature, anti-fouling properties, temperature resistance and corrosion resistance.
The invention has the beneficial effects that:
the titanium metal soft substance can be added into the epoxy resin, so that the glass transition temperature of the epoxy resin can be increased from 80 ℃ to more than 200 ℃, and no substance which can remarkably increase the glass transition temperature of the epoxy resin is found so far; the titanium-based metal soft substance is added into the epoxy resin coating to endow the coating with anti-scaling performance; the titanium metal soft substance can also obviously improve the temperature resistance and the corrosion resistance of the coating.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
In the following examples and comparative examples, parallel tests of the same operation were conducted unless otherwise specified. The modified vinyl ester resin is xinco-221 type modified vinyl ester resin which is purchased from Qitai Xin Ke nanometer new material science and technology development company Limited. The fatty alcohol polyoxypropylene ether S-60 is purchased from Heisen chemical Limited. The specific surface area of the graphene oxide is more than or equal to 50m2(ii) in terms of/g. The dispersion solubilizer S is purchased from Jiangsu Haian petrochemical plants. What is needed isThe type 201 titanate coupling agent is available from Nanjing Temeng chemical Co. The vulcanizing agent bis 25 and the DCP are purchased from Dongguan eucalyptus silica gel science and technology Co., Ltd; the polyacrylamide, Efka LP-9009, BEVLOID6721 are available from Efka corporation; the 202P, 6900-20X, 4400-20X were purchased from DE modest corporation.
In the following examples and comparative examples, the purity of the titanium sponge powder is 99.4%, and the fineness is 120-200 meshes. The disperser is an ESJ-500 type high-speed disperser and is purchased from Shanghai Yile electromechanical equipment Co.
Example 1
A, 100g of titanium sponge powder, 5g of a crushing agent (epoxy resin F51), 5g of a co-crushing agent (sulfur-containing rubber Lp121 type polysulfide rubber), 0.5g of a dispersing agent (HT5168) and 300g of a soft substance carrier (xylene) are taken and dispersed at a high speed of 500r/min in a dispersion machine;
b, taking 500g of the product obtained in the step A, filling the product into a material tank of a high-energy planetary crusher, crushing for 4h, and pouring out to obtain a titanium-based soft substance primary polymer;
and C, taking 500g of the product (titanium-based soft substance initial polymer) obtained in the step B, adding 0.5g of a flocculant (polyacrylamide), 0.1g of a precipitation inhibitor (stearic acid) and 2.5g of a precipitation inhibitor (white carbon black R972), uniformly stirring, filling into a horizontal ball mill, carrying out colloid treatment for 2 hours, and pouring out to obtain the colloid type titanium-based metal soft substance.
Example 2
A, 100g of titanium hydride powder, 10g of a grinding agent (epoxy resin E51), 10g of a co-grinding agent (natural rubber), 0.1g of a dispersing agent (HT-5168) and 300g of a soft substance carrier (coupling agent 501) are taken, and are dispersed at a high speed of 500r/min in a dispersion machine;
b, taking 500g of the product obtained in the step A, filling the product into a material tank of a high-energy planetary crusher, crushing for 3h, and pouring out to obtain a titanium-based soft substance primary polymer;
and C, taking 500g of the product (titanium-based soft substance initial polymer) obtained in the step B, adding 0.1g of anti-flocculant polyacrylamide, 0.2g of anti-precipitation agent (stearic acid) and 2.5g of anti-precipitation agent (BYK410), uniformly stirring, placing into a horizontal ball mill for colloidization for 3 hours, and pouring out to obtain the colloidal titanium-based soft substance.
Example 3
A, 100g of alloy titanium powder, 5g of a crushing agent (5g of epoxy resin E51+5gLp121), 5g of a grinding aid (natural rubber), 0.5g of a dispersing agent (HT-5083) and 300g of a soft matter carrier crosslinking agent (industrial triallyl isocyanurate, CAIT) are taken, and are dispersed at a high speed of 500r/min in a dispersion machine;
b, taking 500g of the product obtained in the step A, filling the product into a charging bucket of a high-energy planetary crusher, crushing for 6 hours, and pouring out to obtain a titanium-based soft substance primary polymer;
and C, taking 500g of the product (titanium-based soft substance initial polymer) obtained in the step B, adding 0.2g of an anti-flocculant (oily amine sulfonate), 0.2g of an anti-precipitation agent (oleic acid) and an anti-precipitation agent (3g of BYK410+1g of white carbon black R972), uniformly stirring, filling into a horizontal ball mill, carrying out colloid treatment for 4 hours, and pouring out to obtain a colloid type titanium-based soft substance.
Experimental example 1
50g of the titanium metal soft substance obtained in the example was added with epoxy resin E44250 g and epoxy resin E20250 g, and further with 8g of silicon carbide and 78g of diphenyl phthalate, and further with 150g of a filler and 214g of a mixed solvent to prepare a paint.
The coating has the following characteristics:
experiments show that 1, the glass transition temperature of the epoxy resin can be increased from 80 ℃ to over 200 ℃ by adding the titanium metal soft substance into the epoxy resin, and no substance which can remarkably increase the glass transition temperature of the epoxy resin is found so far; 2. the coating of the epoxy resin coating prepared by adding the titanium-based metal soft substance has the anti-scaling performance; 3. the temperature resistance and the corrosion resistance of the coating can be obviously improved.
The large industrial application proves that the anti-scaling coating added with the titanium metal soft substance can ensure that a heat exchanger of an oil refinery does not scale for 8 years and does not reduce the heat exchange efficiency; the coating can be used for preventing scaling of an oil field water injection pipe, and can not be scaled after being used for 5 years. The service temperature of the epoxy resin is not more than 80 ℃, and the boiling water tank is free of corrosion and scaling for 5 years after the titanium metal soft substance is added; the general epoxy phenolic aldehyde anticorrosive paint is soaked in a 30% H2S04 solution for 400 hours and then rusted, is soaked in a 10% NaOH solution for 600 hours and then a paint film falls off, and is sprayed for 300 hours in a salt spray test and then rusted; the paint film of the epoxy resin anticorrosive paint added with the titanium nano soft substance is respectively tested for 4320, 6000 and 2000 hours, and the phenomena of discoloration, bubbling, wrinkling, falling, rusting and the like do not occur. The anti-corrosion paint film of the paint has good acid, alkali and salt spray resistance, and is obviously superior to epoxy phenolic aldehyde anti-corrosion paint.
It is used as primer and has far better performance than cold zinc plating, hot zinc spraying and zinc-rich primer. See table 1.
TABLE 1
While the preferred embodiments and examples of the present invention have been described in detail, the present invention is not limited to the embodiments and examples, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (10)
1. A metal soft substance is prepared from the following components:
titanium powder with metal content more than 99.5%, a crushing agent and a disintegrating aid, a dispersing agent, a soft substance carrier, an anti-flocculating agent, an anti-precipitation agent and an anti-precipitation agent;
preferably, the composition by weight is:
a crushing agent and a crushing aid which account for 5-10% of the titanium powder;
a dispersant accounting for 0.5-3% of the titanium powder;
soft matter carrier accounting for 100-500% of the titanium powder;
anti-flocculating agent accounting for 0.02-0.2% of the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft matter carrier;
0.02-0.1% of a precipitation preventing agent accounting for the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft substance carrier;
and
and the anti-settling agent accounts for 0.2-1% of the total amount of the titanium powder, the crushing agent, the crushing assistant, the dispersing agent and the soft matter carrier.
2. The metal soft mass according to claim 1, wherein the titanium powder is selected from one or more of titanium sponge powder, titanium hydride powder and alloy titanium powder.
3. The metal soft matter according to claim 1 or 2, wherein the pulverizing agent is selected from one or more of epoxy resin and sulfur-containing rubber.
4. The metallic soft matter according to any one of claims 1 to 3, wherein the pulverization assisting agent is one or more selected from a silicon coupling agent and a titanate coupling agent.
5. The metal soft mass according to any of claims 1 to 4, wherein the dispersant is selected from one or more of HT-5168 and HT-5083.
6. The metallic soft material of any one of claims 1-5, wherein the soft material carrier is selected from one or more of a solvent, a reactive diluent, and a polymeric cross-linking agent;
and/or the anti-flocculant is selected from one or more of polyacrylamide and oily amine sulfonate;
and/or the anti-precipitation agent is selected from one or more of oleic acid and stearic acid;
and/or the anti-precipitation agent is selected from one or more of white carbon black R972 and BYK 410.
7. A method for producing a metal soft substance according to any one of claims 1 to 6, comprising the steps of:
s01, mixing titanium powder with a crushing agent, a grinding aid, a dispersing agent and a soft matter carrier, and grinding to obtain a titanium-based soft matter primary polymer;
s02, mixing the soft substance primary polymer with a flocculant, a precipitation preventing agent and a precipitating agent, and carrying out colloid treatment to obtain a colloid type titanium-based metal soft substance;
preferably, the milling is carried out in a pulverizer, preferably a high energy planetary pulverizer;
preferably, the peptization treatment is carried out in a ball mill.
8. The method of claim 7, wherein step S01 is preceded by determining the amount of co-crusher to add by testing;
the auxiliary crushing agent can be used for accelerating crushing of reaction substances and increasing the contact area of the reaction, wherein the auxiliary crushing agent can increase or decrease the addition amount according to the reaction speed in a test;
firstly, adding a certain amount of pulverization aid with a preset dosage into an equivalent reactant for testing, and obtaining the test heat change according to the following formula;
wherein mu is the variation of test heat quantity, c is the specific heat capacity of the titanium powder, t is the test time, M is the quantity of the added titanium powder, M is the residual quantity of the titanium powder after the test time t, and RwIn order to form the heat change of the titanium-based soft substance initial polymer, Vs is the volume of a container for mixing the titanium powder, the grinding agent, the grinding aid, the dispersing agent and the soft substance carrier,
(ii) a change in heat upon release of the soft material for said soft material carrier f: (i) As a function of the heat release of the crushing agent, the grinding aid and the dispersing agent,1the amount of the grinding agent is expressed,2the amount of the pulverization aid is expressed,3represents the portion of the dispersant;
then, judging the speed of the reaction according to the test heat;
when the test heat is equal to or larger than a preset value, outputting a prompt for reducing the usage amount of the grinding aid agent on the basis of the preset usage amount to preset electronic equipment;
and when the test heat is smaller than a preset value, outputting a prompt of increasing the usage amount of the grinding aid agent on the basis of the preset usage amount to preset electronic equipment.
9. A resin comprising the metallic soft substance according to any one of claims 1 to 6.
10. Use of a metal soft substance according to any one of claims 1 to 6 for improving resin properties;
preferably, the resin is an epoxy resin;
preferably, the properties include glass transition temperature, anti-fouling properties, temperature resistance and corrosion resistance.
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