CN112175160A - Preparation method of high-strength clean agricultural ground roller adhesive - Google Patents
Preparation method of high-strength clean agricultural ground roller adhesive Download PDFInfo
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- CN112175160A CN112175160A CN202011093372.5A CN202011093372A CN112175160A CN 112175160 A CN112175160 A CN 112175160A CN 202011093372 A CN202011093372 A CN 202011093372A CN 112175160 A CN112175160 A CN 112175160A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/60—Polyamides or polyester-amides
- C08G18/603—Polyamides
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01B—SOIL WORKING IN AGRICULTURE OR FORESTRY; PARTS, DETAILS, OR ACCESSORIES OF AGRICULTURAL MACHINES OR IMPLEMENTS, IN GENERAL
- A01B29/00—Rollers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2310/00—Agricultural use or equipment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Soil Sciences (AREA)
- Environmental Sciences (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of a high-strength clean agricultural ground roller adhesive, belonging to the technical field of high polymer materials.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a preparation method of high-strength clean agricultural ground roller glue.
Background
Soil preparation implements for crushing compacted soil after raking are round rollers made of stone. The roller is called land axle in "the Chinese Yao Shu", and the roller is called the roller in Tang Dynasty. In the Wangzhen nong Shu, the roller is used to speed up the roller, which is usually made of log or round stone roller. The stone roller has no teeth, small holes are respectively chiseled in the centers of two ends of the stone roller, and a short shaft is inserted in the holes or grooves on two ends of rectangular external frame. In nearly a hundred years, the roller has been eliminated after the thresher, the roller has been left out of the farm-ploughed stage, the people who have entered the comfortable society at present have almost not used it, the features have been moved to the place where people gather in the door or the village, when sitting on the couch or dining table, they continue to play their roles, in modern agricultural machinery, the roller having the same function as the roller is still used, but wooden and stone ground rollers have poor durability, are easy to damage and heavy, are easy to breed mold due to slime and rot, and size, weight are difficult to adapt to the agricultural production of technology parameterization, and the ground roller is the necessary simple and practical instrument of peasant household, and the machine is supporting, can cut up again when loosening the soil and bury the root stubble below the earth's surface and go with base fertilizer application to soil, and the rearmounted ground roller that presses on the machines flattens soil, plays the effect of keeping plucking, promotes the effect of dark loose soil preparation technique: one is to effectively and thoroughly break the hard plough layer formed in the long years. The traditional ploughing mode can be changed by the mechanical deep scarification depth, the original plough base layer is broken, the proportion of the live soil layer is increased, the soil tilth is improved, the original plough base is kept, and the simple land pressing roller has an important role in planting crops such as vegetables, soybeans, corns, and the like, for example, Chinese patent CN103891434A discloses a straw return roller press with good land pressing effect, Chinese patent CN206879358U discloses a squirrel cage type soil crushing and land pressing roller, Chinese patent CN109289965A discloses a machine with rollers capable of moving relatively, in addition, the land pressing roller is also an important part of various agricultural machinery, such as a mulching film integrated planting machine, the service performance of the existing land pressing roller is poor, and technicians in the field need to develop a preparation method of high-strength clean land pressing roller glue for agricultural use urgently to meet the existing use requirements.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a high-strength clean agricultural ground roller adhesive.
A preparation method of high-strength clean agricultural ground roller glue comprises the following steps:
(1) melting 100 parts of caprolactam at 90-100 ℃, performing vacuum dehydration for 20-30 min, adjusting the temperature to 100-130 ℃, adding 0.6-0.8 part of potassium hydroxide, adjusting the temperature to 90-100 ℃, performing vacuum dehydration for 20-30 min, adding 5-10 parts of toluene diisocyanate, and uniformly stirring to obtain a prepolymer; (2) preparing a reinforcing filler: under the protection of light and nitrogen, mixing 13-14 parts by weight of formaldehyde aqueous solution with the mass fraction of 37% with 20-21 parts by weight of phenol, adding 45-53 parts by weight of nano halloysite nanotube, mechanically stirring for 20-30 min, adjusting the temperature to 90-100 ℃, adding 0.2-0.3 part by weight of oxalic acid hydrate, stirring for catalytic reaction for 20-30 min, washing with deionized water and absolute ethyl alcohol for multiple times, filtering, drying, grinding and sieving to obtain phenolic aldehyde modified halloysite; (3) preparing a ground roller: completely melting the prepolymer obtained in the step (1) at 90-130 ℃, adding 35-40 parts of phenolic aldehyde modified halloysite, and dispersing for 10-100 min under the synergistic action of ultrasonic waves; adjusting the temperature to 125-150 ℃, distilling under reduced pressure to remove water, then adding 1-3 parts of an alkali catalyst into the reaction kettle, performing vacuum distillation to remove water again, adjusting the temperature to 135-160 ℃, removing vacuum, rapidly adding 1-3 parts of a polyisocyanate activating agent, uniformly stirring, rapidly injecting into a mold preheated to 160-200 ℃, performing polymerization for 10-20 minutes, naturally cooling, and demolding.
Further, the alkali catalyst in the step (3) is any one of urotropine, metal potassium, sodium hydroxide, sodium caprolactam and sodium methoxide.
Further, the synergistic ultrasonic dispersion is ultraviolet light and microwave synergistic ultrasonic dispersion, wherein the wavelength of the ultraviolet light is 320-350 nm, the frequency of the ultrasonic wave is 10-20 kHz, and the frequency of the microwave is 2450-2500 MHz.
Further, the polyisocyanate activating agent in the step (3) is any one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate and triphenylmethane triisocyanate.
Further, the nanometer halloysite nanotube obtained in the step (2) is sieved by a 100-mesh sieve, then is placed in a constant temperature box at 60 ℃ for drying for 12-14 h, and then is roasted in a muffle furnace at 550-600 ℃ for 1-2 h.
The invention has the beneficial effects that:
the halloysite nanotube used in the preparation method disclosed by the invention is a natural silicate clay mineral, and mainly exists in nature in the form of the nanotube; the phenolic aldehyde modified halloysite is a mesoporous material, is very suitable for serving as a carrier of heterogeneous catalytic reaction, promotes the polymerization of caprolactam, improves the strength of roller glue, plays the role of a nucleating agent when nylon is polymerized and molded, can form a uniform, fine and dense crystal structure in a cooling process, improves the crystallinity, enhances the surface hardness, reduces the abrasion, reduces the thermal expansion friction process, can promote the components of the modified nylon to be preferentially transferred to a shaft neck under the action of frictional heat energy to form a tough and wear-resistant lubricating film, forms the friction between the modified nylon and the transferring film, improves the friction surface state, obtains good self-lubrication, and realizes the application performance, the soil adhesion resistance and the lubricating performance of the ground roller, The dimensional stability is improved.
Compared with the prior art, the invention has the following advantages:
the high-strength clean agricultural land roller adhesive prepared by the preparation method disclosed by the invention has the advantages of good lubricating property, long service life, light weight, convenience in installation and the like, has good high strength and toughness, is simple in preparation process equipment and mould, good in mechanical property, shock-absorbing, wear-resistant, self-lubricating, corrosion-resistant, wide in use temperature range and good in economic benefit.
Detailed Description
Example 1
(1) Melting 100 parts of caprolactam at 100 ℃, carrying out vacuum dehydration for 30min, adjusting the temperature to 130 ℃, adding 0.8 part of potassium hydroxide, adjusting the temperature to 100 ℃, carrying out vacuum dehydration for 30min, finally adding 10 parts of toluene diisocyanate, and uniformly stirring to obtain a prepolymer; (2) preparing a reinforcing filler: under the protection of light and nitrogen, mixing 14 parts by weight of formaldehyde aqueous solution with the mass fraction of 37% with 21 parts by weight of phenol, adding 53 parts by weight of nano halloysite nanotube, mechanically stirring for 30min, adjusting the temperature to 100 ℃, adding 0.3 part by weight of oxalic acid hydrate, stirring for catalytic reaction for 30min, washing with deionized water and absolute ethyl alcohol for multiple times, filtering, drying, grinding and sieving to obtain phenolic aldehyde modified halloysite; (3) preparing a ground roller: completely melting the prepolymer obtained in the step (1) at 130 ℃, adding 40 parts of phenolic aldehyde modified halloysite, and performing synergistic ultrasonic dispersion to obtain ultraviolet light and microwave synergistic ultrasonic dispersion, wherein the ultraviolet light has the wavelength of 350nm, the ultrasonic frequency of 20kHz and the microwave frequency of 2500MHz and is dispersed for 100 min; adjusting the temperature to 150 ℃, distilling under reduced pressure to remove water, then adding 3 parts of alkali catalyst urotropine into the reaction kettle, carrying out vacuum distillation to remove water again, adjusting the temperature to 160 ℃, removing vacuum, rapidly adding 3 parts of isophorone diisocyanate, stirring uniformly, rapidly injecting into a mold preheated to 200 ℃, carrying out polymerization reaction for 20 minutes, naturally cooling, and demolding, sieving the nanometer halloysite nanotube obtained in the step (2) with a 100-mesh sieve, then placing in a 60 ℃ constant temperature box for drying for 14 hours, and then roasting in a 600 ℃ muffle furnace for 2 hours.
Example 2
(1) Melting 100 parts of caprolactam at 90 ℃, carrying out vacuum dehydration for 20min, adjusting the temperature to 100 ℃, adding 0.6 part of potassium hydroxide, cooling to 90 ℃, carrying out vacuum dehydration for 20min, finally adding 5 parts of toluene diisocyanate, and uniformly stirring to obtain a prepolymer; (2) preparing a reinforcing filler: under the protection of light and nitrogen, mixing 13 parts by weight of formaldehyde aqueous solution with the mass fraction of 37% with 20 parts by weight of phenol, adding 45 parts by weight of nano halloysite nanotube, mechanically stirring for 20min, adjusting the temperature to 90 ℃, adding 0.2 part by weight of oxalic acid hydrate, stirring, catalyzing and reacting for 20min, washing with deionized water and absolute ethyl alcohol for multiple times, filtering, drying, grinding and sieving to obtain phenolic aldehyde modified halloysite; (3) preparing a ground roller: completely melting the prepolymer obtained in the step (1) at 90 ℃, adding 35 parts of phenolic aldehyde modified halloysite, and dispersing by ultraviolet light and microwave in cooperation with ultrasonic waves, wherein the wavelength of the ultraviolet light is 320nm, the frequency of the ultrasonic waves is 10kHz, and the frequency of the microwave is 2450MHz, and dispersing for 10min in cooperation with the ultrasonic waves; adjusting the temperature to 125 ℃, distilling under reduced pressure to remove water, then adding 1 part of sodium methoxide serving as an alkali catalyst into the reaction kettle, performing vacuum distillation again to remove water, adjusting the temperature to 135 ℃, removing vacuum, rapidly adding 1 part of hexamethylene diisocyanate serving as an activator, uniformly stirring, rapidly injecting into a mold preheated to 160 ℃, performing polymerization reaction for 10 minutes, naturally cooling, and demolding, wherein the nano halloysite nanotube obtained in the step (2) passes through a 100-mesh sieve, then drying in a constant temperature box at 60 ℃ for 12 hours, and then roasting in a muffle furnace at 550 ℃ for 1 hour.
Comparative example 1
In this comparative example, compared with example 2, in the step (1), the phenolic-modified halloysite component was omitted, except that the process steps were the same.
Comparative example 2
This comparative example compares to example 2 in step (1), the polyisocyanate activator component is omitted, except that the process steps are the same.
Comparative example 3
This comparative example compares to example 2 in that in step (3) the phenolic modified halloysite was replaced with untreated nano-halloysite nanotubes, except that the process steps were otherwise the same.
Comparative example 4
This comparative example compares to example 2 in that in step (3) the prepolymer is replaced by caprolactam, except that the process steps are otherwise identical.
The performance of the high-strength clean agricultural pressure roller adhesive of the embodiments 1-2 and the comparative examples 1-4 is tested, and the test results are shown in Table 1
TABLE 1 Performance test results of high-strength clean agricultural roller adhesive for ground roller in each example and comparative example
| Item | Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Elongation at break% | 12.5% | 13.4% | 12.1% | 12.4% | 12.6% | 12.8% |
| Coefficient of friction | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
| Water absorption% | 0.9% | 0.9% | 0.9% | 0.9% | 0.9% | 0.9% |
| Simple supported beam gapless impact strength kJ/m2 | 65.3 | 67.4 | 64.3 | 63.8 | 63.7 | 64.1 |
| Tensile strength MPa | 80.8 | 79.6 | 78.5 | 76.5 | 79.6 | 77.8 |
| Compressive strength MPa | 112.4 | 112.5 | 112.9 | 111.0 | 110.8 | 112.6 |
| Bending strength MPa | 141.3 | 142.3 | 139.0 | 139.3 | 138.4 | 137.8 |
| 1.81MPa load deformation temperature DEG C | 119.6 | 120.4 | 116.6 | 115.3 | 118.9 | 115.8 |
| Hardness MPa | 124.8 | 125.6 | 123.1 | 120.6 | 120.0 | 124.3 |
Note: the density is regulated according to GB/T1033.1-2008; the water absorption is carried out according to the measurement regulation of GB/T1034-2008 plastic water absorption; tensile strength and elongation at break were determined according to GB/T1040.1-2018 tensile Properties of plastics part 1: the process is specified; the bending strength is measured according to the GB/T9341-2008 plastic bending performance measurement regulation, and the compressive strength is measured according to the GB/T1041-2008 plastic compressive performance measurement regulation; impact strength was determined according to GB/T1043.1-2008 Plastic simple Supports impact Performance part 1: performing non-instrumented impact test regulation; the hardness is measured according to GB/T3398.1-2008 plastic hardness: part 1: the ball indentation method is specified; heat distortion temperature determination according to GB/T1634.1-2019 part 1 of Plastic load distortion temperature: the general test method is specified; the friction coefficient is carried out according to the specification of a GB3960-2016 plastic sliding friction wear test method; the linear expansion coefficient is determined according to the quartz expansion method for determining the linear expansion coefficient of GB/T1036-2008 plastic at-30 ℃.
Claims (5)
1. A preparation method of high-strength clean agricultural ground roller glue is characterized by comprising the following steps:
(1) melting 100 parts of caprolactam at 90-100 ℃, performing vacuum dehydration for 20-30 min, adjusting the temperature to 100-130 ℃, adding 0.6-0.8 part of potassium hydroxide, adjusting the temperature to 90-100 ℃, performing vacuum dehydration for 20-30 min, adding 5-10 parts of toluene diisocyanate, and uniformly stirring to obtain a prepolymer; (2) preparing a reinforcing filler: under the protection of light and nitrogen, mixing 13-14 parts by weight of formaldehyde aqueous solution with the mass fraction of 37% with 20-21 parts by weight of phenol, adding 45-53 parts by weight of nano halloysite nanotube, mechanically stirring for 20-30 min, adjusting the temperature to 90-100 ℃, adding 0.2-0.3 part by weight of oxalic acid hydrate, stirring for catalytic reaction for 20-30 min, washing with deionized water and absolute ethyl alcohol for multiple times, filtering, drying, grinding and sieving to obtain phenolic aldehyde modified halloysite; (3) preparing a ground roller: completely melting the prepolymer obtained in the step (1) at 90-130 ℃, adding 35-40 parts of phenolic aldehyde modified halloysite, and dispersing for 10-100 min under the synergistic action of ultrasonic waves; adjusting the temperature to 125-150 ℃, distilling under reduced pressure to remove water, then adding 1-3 parts of an alkali catalyst into the reaction kettle, performing vacuum distillation to remove water again, adjusting the temperature to 135-160 ℃, removing vacuum, rapidly adding 1-3 parts of a polyisocyanate activating agent, uniformly stirring, rapidly injecting into a mold preheated to 160-200 ℃, performing polymerization for 10-20 minutes, naturally cooling, and demolding.
2. The method for preparing a high-strength clean agricultural roller press glue according to claim 1, wherein the base catalyst in step (3) is any one of urotropine, metal potassium, sodium hydroxide, sodium caprolactam and sodium methoxide.
3. The preparation method of the high-strength cleaning agricultural land roller adhesive as claimed in claim 1, wherein the synergistic ultrasonic dispersion is ultraviolet light and microwave synergistic ultrasonic dispersion, wherein the wavelength of the ultraviolet light is 320-350 nm, the frequency of the ultrasonic wave is 10-20 kHz, and the frequency of the microwave is 2450-2500 MHz.
4. The method for preparing a high-strength clean agricultural roller adhesive according to claim 1, wherein the polyisocyanate activating agent of the step (3) is any one of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate and triphenylmethane triisocyanate.
5. The preparation method of the high-strength clean agricultural roller adhesive for the ground pressure as claimed in claim 1, wherein the nano halloysite nanotubes obtained in the step (2) are sieved by a 100-mesh sieve, then are dried in a 60 ℃ thermostat for 12-14 h, and then are roasted in a 550-600 ℃ muffle furnace for 1-2 h.
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| CN202011093372.5A CN112175160A (en) | 2020-10-14 | 2020-10-14 | Preparation method of high-strength clean agricultural ground roller adhesive |
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| CN202011093372.5A CN112175160A (en) | 2020-10-14 | 2020-10-14 | Preparation method of high-strength clean agricultural ground roller adhesive |
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Application publication date: 20210105 |
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