CN114479999B - Lubricating oil for rapid dehydration papermaking circulation system - Google Patents

Lubricating oil for rapid dehydration papermaking circulation system Download PDF

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Publication number
CN114479999B
CN114479999B CN202210027085.7A CN202210027085A CN114479999B CN 114479999 B CN114479999 B CN 114479999B CN 202210027085 A CN202210027085 A CN 202210027085A CN 114479999 B CN114479999 B CN 114479999B
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lubricating oil
percent
water
placing
papermaking
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CN114479999A (en
Inventor
许宏涛
许群益
蒋华良
单秀华
潘峻
丁艺博
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Jiangsu Zhongsheng High Tech Environment Co ltd
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Jiangsu Zhongsheng High Tech Environment Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/04—Mixtures of base-materials and additives
    • C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
    • B01J20/3057—Use of a templating or imprinting material ; filling pores of a substrate or matrix followed by the removal of the substrate or matrix
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
    • C10G25/06—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents with moving sorbents or sorbents dispersed in the oil
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    • C10G2300/10—Feedstock materials
    • C10G2300/1037—Hydrocarbon fractions
    • C10G2300/1062—Lubricating oils
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    • C10G2300/20—Characteristics of the feedstock or the products
    • C10G2300/201—Impurities
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    • C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
    • C10G2400/10—Lubricating oil
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    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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    • C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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    • C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
    • C10M2203/102—Aliphatic fractions
    • C10M2203/1025—Aliphatic fractions used as base material
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    • C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
    • C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
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    • C10N2060/10—Chemical after-treatment of the constituents of the lubricating composition by sulfur or a compound containing sulfur
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The invention provides a lubricating oil for a rapid dehydration papermaking circulation system, which comprises the following components: poly alpha-olefin, dehydrating agent, lauric acid diethanolamide, defoaming agent, alkylamine and ethylene oxide condensate, extreme pressure antiwear agent, flame retardant, anti-aging agent, high temperature resistant antioxidant, copper corrosion inhibitor, carbodiimide, corrosion inhibitor, 500N base oil and 150BS base oil mixture. The invention provides a method for preparing a rapid dehydration papermaking circulation system lubricating oil by using barium dinonylnaphthalene sulfonate and dodecenylsuccinic acid with rapid dehydration as a synergistic dehydration functional material and then matching with a filter aid, namely lauric acid diethanolamide and other functional additives.

Description

Lubricating oil for rapid dehydration papermaking circulation system
Technical Field
The invention relates to the technical field of lubricating oil, in particular to lubricating oil for a rapid dehydration papermaking circulation system.
Background
The lubrication of a papermaking circulating system is a typical mixed lubrication system, which integrates gear oil, hydraulic oil and hydraulic transmission oil into a whole, and meanwhile, the working temperature is higher, and a large amount of water is inevitably contacted. Products in the current market, including synthetic products, generally have low dehydration speed, cause water-carrying lubrication in different degrees, easily cause poor lubrication and shorten the oil change period. As a pollutant in lubricating oil, water not only can influence the physicochemical properties of oil products to cause a series of abnormal oil decay, but also can influence the normal operation of the whole lubricating system to cause lubricating faults of different degrees and cause huge economic loss. At present, in the aspect of lubricating oil dehydration and purification, sufficient attention is not paid, the main reason is insufficient understanding of harm of water pollution, and when the water content in oil is low, sudden accidents such as blocking and the like (emergency stop accidents can be caused when the water content is serious) cannot be caused. In fact, the deterioration of the oil properties caused by water pollution leads to wear of the components (including chemical corrosion, generating substances that affect the operation) which is not inferior to the effect of particle pollution on the system. Oil with serious particle pollution can be recycled through filtration and purification treatment, and the oil deterioration caused by water pollution can also cause the scrapping of a large amount of oil products.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems that the existing papermaking circulation system inevitably contacts a large amount of water during operation, so that water-carrying lubrication with different degrees is caused, poor lubrication is easy to occur, the oil change period is shortened, and even an emergency stop accident is caused, the invention provides the rapid dehydration papermaking circulation system lubricating oil which is obtained by adopting barium dinonylnaphthalene sulfonate and dodecenylsuccinic acid with rapid dehydration as synergistic dehydration functional materials and matching with filter aid lauric acid diethanolamide and other functional additives.
The technical scheme is as follows: a rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight:
Figure BDA0003465091350000011
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Figure BDA0003465091350000021
preferably, the volume ratio of the 500N base oil to the 150BS base oil is 1 (3-5).
Preferably, the defoaming agent is methyl silicone oil ester or/and fluorine-containing silicone oil; the extreme pressure antiwear agent is one or more of sulfurized isoolefin, amino thioester and isooctyl acid phospholipid octadecyl amine; the flame retardant is di-n-butyl phosphite and/or tricresyl phosphate.
Preferably, the dehydrating agent comprises a main dehydrating agent and an auxiliary dehydrating agent, the mass ratio of the main dehydrating agent to the auxiliary dehydrating agent is 5.
Preferably, the preparation method of the primary dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
Preferably, the preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then performing ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Preferably, the anti-aging agent is 2,2 '-methylenebis (4-ethyl-6-tert-butylphenol) and/or 4,4' -methylenebis (2, 6-di-tert-butylphenol).
Preferably, the high-temperature-resistant antioxidant is one or more of alkyl diphenylamine, octylbutyl diphenylamine and p, p-diisooctyldiphenyl amine.
Preferably, the corrosion inhibitor is benzotriazole and/or methylbenzotriazole.
Preferably, the copper corrosion inhibitor is an N, N' -dialkylaminomethylenephriazole and/or a benzotriazole-aldehyde-amine condensate.
Has the advantages that:
1. according to the invention, barium dinonyl naphthalene sulfonate and dodecenyl succinic acid with a rapid dehydration function are used as a synergistic dehydration functional material, and then are matched with a filter aid, namely lauric acid diethanolamide and other functional additives, so that the lubricating oil of a rapid dehydration papermaking circulation system can be obtained.
2. The multi-stage porous carbon prepared by the invention is treated by nitric acid to obtain hydrogen in nitric acid, and nitrogen atoms in barium dinonyl naphthalene sulfonate molecules contain lone-pair electrons and can be firmly combined with hydrogen in acid molecules by hydrogen bonds, so that the barium dinonyl naphthalene sulfonate is firmly combined on the multi-stage porous carbon.
3. The multi-stage porous carbon adopted by the invention has a micropore-mesopore structure and a high specific surface area, improves the density and stability of the barium dinonyl naphthalene sulfonate, increases the number of effective active sites, and overcomes the defects of non-uniform dispersion, poor dehydration effect and incapability of recycling caused by directly using the barium dinonyl naphthalene sulfonate.
4. The lubricating oil for the rapid dehydration papermaking circulating system can overcome the defects of the conventional product, improves the dehydration property, strengthens the lubricating and protecting capabilities, and does not influence the filterability.
5. The invention may also be applied in mineral oil formulations and synthetic formulations.
Detailed Description
Example 1
A rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.1%; the main dehydrating agent and the dodecenylsuccinic acid are 2.0 percent, and the mass ratio of the main dehydrating agent to the dodecenylsuccinic acid is 5; lauric acid diethanolamide 0.5%; methyl silicone oil ester 5.0ppm; alkylamine condensate with ethylene oxide 5.0ppm; 1.0% of sulfurized isoolefin; 1.0 percent of dibutyl phosphite; 2,2' -methylenebis (4-ethyl-6-tert-butylphenol) 0.3; 0.2 parts of alkyl diphenylamine; 0.1% of N, N' -dialkylaminomethylene benzotriazole; 0.5% of carbodiimide; 0.02% of benzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1.
The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h at the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, calcining in a muffle furnace at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then performing ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Example 2
A rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.2%; 3.0 percent of main dehydrating agent and 3.0 percent of dodecenylsuccinic acid, wherein the mass ratio of the main dehydrating agent to the dodecenylsuccinic acid is 5; 1.0% of lauric acid diethanolamide; 10.0ppm of fluorine-containing silicone oil; alkylamine and ethylene oxide condensate 10.0ppm; 1.5% of aminothioester; 1.5% of tricresyl phosphate; 0.5 percent of 4,4' -methylene bis (2, 6-di-tert-butylphenol); 0.4 percent of octyl butyl diphenylamine; benzotriazole-aldehyde-amine condensate 0.3%; 0.6 percent of carbodiimide; 0.04 percent of methylbenzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1.
The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in an autoclave, crystallizing for 72 hours at 150 ℃, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Is placed at 1.8mol/LNH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then performing ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Example 3
A rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.3%; 4.0 percent of main dehydrating agent and 4.0 percent of dodecenylsuccinic acid, wherein the mass ratio of the main dehydrating agent to the dodecenylsuccinic acid is 5; 1.5 percent of lauric acid diethanolamide; methyl silicone oil ester 10.0ppm; alkylamine and ethylene oxide condensate 10.0ppm; 2.0 percent of isooctyl acid sulfur and phosphorus ester octadecylamine; 1.5 percent of dibutyl phosphite; 0.7 percent of 2,2' -methylene-bis (4-ethyl-6-tert-butyl phenol); 0.6 percent of p, p-diisooctyl diphenylamine; 0.5 percent of N, N' -dialkylaminomethylene benzotriazole; 0.8% of carbodiimide; 0.05 percent of benzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1. The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder in a small amount for multiple times under the stirring condition, performing ultrasonic treatment for 1h, continuously stirring for 2h, placing into an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain the multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then performing ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Example 4
A rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.4%; 5.0 percent of main dehydrating agent and 5.0 percent of dodecenylsuccinic acid, wherein the mass ratio of the main dehydrating agent to the dodecenylsuccinic acid is 5; lauric acid diethanolamide 2.0%; 10.0ppm of fluorine-containing silicone oil; alkylamine and ethylene oxide condensate 10.0ppm; 2.5 percent of sulfurized isoolefin; 1.5 percent of di-n-butyl phosphite; 0.9 percent of 4,4' -methylene bis (2, 6-di-tert-butylphenol); 0.8 percent of alkyl diphenylamine; benzotriazole-aldehyde-amine condensate 0.7%; 0.9% of carbodiimide; 0.07 percent of methylbenzotriazole; the balance of a mixture of 500N base oil and 150BS base oil; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1.
The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain the multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in Cl aqueous solution at 120 deg.C for 1h, and hydrothermal strip at 700 deg.C with 100% water vaporCarrying out under-part ultra-stabilization treatment for 2h;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Example 5
A rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.5%; 6.0 percent of main dehydrating agent and 6.0 percent of dodecenylsuccinic acid, wherein the mass ratio of the main dehydrating agent to the dodecenylsuccinic acid is 5; lauric acid diethanolamide 2.5%; methyl silicone oil ester 15.0ppm; alkylamine and ethylene oxide condensate 15.0ppm; 3.0% of aminothioester; 2.0% of di-n-butyl phosphite; 0.3 to 1.0 percent of 2,2' -methylene bis (4-ethyl-6-tert-butylphenol); 1.0 percent of octyl butyl diphenylamine; 0.8 percent of N, N' -dialkylaminomethylene benzotriazole; 1.0% of carbodiimide; 0.09 percent of benzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1.
The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder in a small amount for multiple times under the stirring condition, performing ultrasonic treatment for 1h, continuously stirring for 2h, placing into an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight; (8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl aluminum oxide, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred continuously for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2 hours to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing the solution in 1.8mol/L of NH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then performing ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Comparative example 1
The difference between this example and example 5 is that dodecenylsuccinic acid, an auxiliary dehydrating agent, is not included, specifically:
a rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.5%; 5.0 percent of primary dehydrating agent; lauric acid diethanolamide 2.5%; methyl silicone oil ester 15.0ppm; alkylamine and ethylene oxide condensate 15.0ppm; 3.0% of aminothioester; 2.0% of di-n-butyl phosphite; 0.3 to 1.0 percent of 2,2' -methylene bis (4-ethyl-6-tert-butylphenol); 1.0 percent of octyl butyl diphenylamine; 0.8 percent of N, N' -dialkylaminomethylene benzotriazole; 1.0% of carbodiimide; 0.09 percent of benzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1. The preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h; (4) Placing in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight;
(8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring to a high-pressure reaction kettle, reacting for 24 hours at 200 ℃, taking out, washing with water and drying to obtain the product.
The preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl aluminum oxide, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred continuously for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in a high-pressure kettle, crystallizing at 150 ℃ for 72h, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in Cl aqueous solution at 120 deg.C for 1h, and hydrothermal reaction at 700 deg.C with 100% water vaporPerforming ultra-stabilization treatment for 2 hours;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
Comparative example 2
This example differs from example 5 in that it does not contain a dehydrating agent, in particular:
a rapid dehydration papermaking circulation system lubricating oil comprises the following components in percentage by weight: poly alpha-olefin 0.5%; lauric acid diethanolamide 2.5%; methyl silicone oil ester 15.0ppm; 15.0ppm of a condensate of alkylamine with ethylene oxide; 3.0% of aminothioester; 2.0% of di-n-butyl phosphite; 0.3 to 1.0 percent of 2,2' -methylene bis (4-ethyl-6-tert-butylphenol); 1.0 percent of octyl butyl diphenylamine; 0.8 percent of N, N' -dialkylaminomethylene benzotriazole; 1.0% of carbodiimide; 0.09 percent of benzotriazole; the balance of a 500N base oil and 150BS base oil mixture; wherein the volume ratio of the 500N base oil to the 150BS base oil is 1.
The water content in the lubricating oil is measured by combining a sound method and a Waltesmo (waters Mo) test paper method:
(1) The sound method comprises the following steps: putting the lubricating oil on a small disc made of aluminum foil or tinfoil, heating at high temperature for l-2min, and if splashing or bubbling occurs, the water content is high; if continuous crackling sound exists, the water content is more than 0.03 percent; if no sound is produced after a little crackle exists, the water content is less than 0.03 percent. (2) Waltsmol (waters Mo) dipstick method: the water content can be determined by immersing the Waltesmo test paper in oil, which shows blue spots when the test paper is in contact with water, as shown in Table 1.
TABLE 1 relationship between specks and water content in oil by Waltsmo test paper method
Number of speckles/piece 1 (Small) 1-2 About 5 About 10
Water content (%) ＜0.5 0.5 1.0 2.0
Table 2 water content of each example in use
Figure BDA0003465091350000101
Research shows that for the lubricating oil of the papermaking circulating system, when the water content reaches 0.1%, the oil begins to turn white and turbid; when the water content reaches 0.8%, the bearings are severely worn. The test result of the four-ball machine shows that the abrasion resistance is gradually reduced along with the increase of the water content; when the water content reaches 2.5%, the abrasion resistance is sharply reduced, and the lubricating property of the lubricating oil of the papermaking circulation system is lost.

Claims (9)

1. The lubricating oil for the rapid dehydration papermaking circulating system is characterized in that: comprises the following components in percentage by weight:
poly alpha-olefin 0-0.5%
2.0 to 6.0 percent of dehydrating agent
Lauric acid diethanolamide 0.5-2.5%
5.0-15.0 ppm of defoaming agent
Alkylamine and epoxyethane condensate 5.0-15.0 ppm
1.0 to 3.0 percent of extreme pressure antiwear agent
1.0 to 2.0 percent of fire retardant
0.3 to 1.0 percent of antiager
0.2 to 1.0 percent of high-temperature resistant antioxidant
0.1 to 0.8 percent of copper corrosion inhibitor
0.5 to 1.0 percent of carbodiimide
0.02 to 0.09 percent of corrosion inhibitor
The balance of a 500N base oil and 150BS base oil mixture;
the dehydrating agent comprises a main dehydrating agent and an auxiliary dehydrating agent, the mass ratio of the main dehydrating agent to the auxiliary dehydrating agent is 5;
the preparation method of the main dehydrating agent comprises the following steps:
(1) Dissolving 2g of molasses in 10g of water, adding 80 mu L of concentrated sulfuric acid, uniformly mixing, and adding a small amount of 1.0g of hierarchical pore molecular sieve for multiple times under the stirring condition;
(2) Performing ultrasonic treatment for 1h, continuing stirring for 2h, placing into an oven, keeping at 100 deg.C for 6h, heating to 160 deg.C for 6h, taking out the solid, and grinding to obtain powder;
(3) Dissolving 0.8g of molasses in 5g of water, adding 50 mu L of concentrated sulfuric acid, uniformly mixing, adding the powder for a few times under the stirring condition, carrying out ultrasonic treatment for 1h, continuously stirring for 2h, placing in an oven, keeping the temperature at 100 ℃ for 6h, and heating to 160 ℃ for 6h;
(4) Placed in a tube furnace, N 2 Carbonizing under the protection of atmosphere;
(5) Mixing the carbonized product with 3mol of sodium hydroxide solution, stirring for 1h according to the solid-liquid mass ratio of 1;
(6) Cooling to room temperature, washing the solid particles with distilled water until the pH value is neutral, and drying to obtain multi-level porous carbon;
(7) Putting 1g of hierarchical porous carbon into 30ml of 20% nitric acid, stirring and soaking at room temperature for 24 hours, filtering and washing, and drying overnight;
(8) Taking out, adding 1g of barium dinonylnaphthalene sulfonate and 30ml of water, uniformly mixing, transferring the mixture into a high-pressure reaction kettle, reacting for 24 hours at the temperature of 200 ℃, taking out, washing with water and drying to obtain the product.
2. The rapid dehydration papermaking cycle system lubricating oil according to claim 1, characterized in that: the volume ratio of the 500N base oil to the 150BS base oil is 1 (3-5).
3. The rapid dewatering papermaking circulation system lubricating oil according to claim 1, characterized in that: the defoaming agent is methyl silicone oil ester or/and fluorine-containing silicone oil; the extreme pressure antiwear agent is one or more of sulfurized isoolefin, amino thioester and isooctyl acidic lecithin octadecylamine; the flame retardant is di-n-butyl phosphite and/or tricresyl phosphate.
4. The rapid dehydration papermaking cycle system lubricating oil according to claim 1, characterized in that: the preparation method of the hierarchical pore molecular sieve comprises the following steps:
(1) 0.1g of isopropyl alumina, 4.5g of dodecyl trimethyl ammonium hydroxide and 30ml of water are taken to be mixed and stirred uniformly, 4.0g of tetraethoxysilane is added, and the mixture is stirred for 1 hour;
(2) Adding 5mL of ethanol solution in which 0.4g of rosinyl carbamate quaternary ammonium salt is dissolved, and continuously stirring for 2h to obtain gel;
(3) Placing the gel in an autoclave, crystallizing for 72 hours at 150 ℃, taking out, naturally cooling, washing with distilled water, and performing suction filtration;
(4) Placing into a drying oven, drying at 100 deg.C for 3 hr, placing into a muffle furnace, calcining at 600 deg.C for 6 hr, and grinding into powder;
(5) Placing in 1.8mol/L NH 4 Reacting in a Cl aqueous solution at 120 ℃ for 1h, and then carrying out ultra-stabilization treatment for 2h under the hydrothermal condition of 700 ℃ and 100% of water vapor;
(6) Roasting in a muffle furnace at 600 ℃ for 4h to obtain the hierarchical pore molecular sieve.
5. The rapid dehydration papermaking cycle system lubricating oil according to claim 1, characterized in that: the anti-aging agent is 2,2 '-methylene bis (4-ethyl-6-tert-butylphenol) and/or 4,4' -methylene bis (2, 6-di-tert-butylphenol).
6. The rapid dewatering papermaking circulation system lubricating oil according to claim 1, characterized in that: the high-temperature-resistant antioxidant is alkyl diphenylamine.
7. The rapid dehydration papermaking cycle system lubricating oil according to claim 6, characterized in that: the alkyl diphenylamine is octyl butyl diphenylamine and/or p, p-diisooctyl diphenylamine.
8. The rapid dehydration papermaking cycle system lubricating oil according to claim 1, characterized in that: the corrosion inhibitor is benzotriazole and/or methylbenzotriazole.
9. The rapid dehydration papermaking cycle system lubricating oil according to claim 1, characterized in that: the copper corrosion inhibitor is N, N' -dialkyl amino methylene benzotriazole and/or benzotriazole-aldehyde-amine condensate.
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