CN111909756A - Gel ink pen refill follow-up sealant and preparation method and application thereof - Google Patents
Gel ink pen refill follow-up sealant and preparation method and application thereof Download PDFInfo
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- CN111909756A CN111909756A CN202010570552.1A CN202010570552A CN111909756A CN 111909756 A CN111909756 A CN 111909756A CN 202010570552 A CN202010570552 A CN 202010570552A CN 111909756 A CN111909756 A CN 111909756A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B43—WRITING OR DRAWING IMPLEMENTS; BUREAU ACCESSORIES
- B43K—IMPLEMENTS FOR WRITING OR DRAWING
- B43K7/00—Ball-point pens
-
- 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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
- C10M2201/1036—Clays; Mica; Zeolites used as thickening agents
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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
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
- C10M2201/145—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds used as thickening agents
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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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/32—Esters of carbonic acid
-
- 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
- C10M2229/00—Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
- C10M2229/04—Siloxanes with specific structure
- C10M2229/041—Siloxanes with specific structure containing aliphatic substituents
- C10M2229/0415—Siloxanes with specific structure containing aliphatic substituents used as base material
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention relates to the technical field of lubricating sealants, in particular to a gel-ink pen refill follow-up sealant and a preparation method and application thereof. The gel ink pen refill follow-up sealing agent comprises silicone oil, organic bentonite and a structure improving agent. The gel ink pen refill follow-up sealant is incompatible with ink, has excellent viscosity, impact resistance, high and low temperature performance and follow-up performance and excellent comprehensive performance, and can be used for gel ink pen refills to play the roles of sealing and liquid pistons.
Description
Technical Field
The invention relates to the technical field of lubricating sealants, in particular to a gel-ink pen refill follow-up sealant and a preparation method and application thereof.
Background
The follow-up sealant of the gel ink pen refill can seal ink in the pen tube, prevent the ink from evaporating or flowing backwards, and follow up the follow-up sealing due to ink reduction in the writing process. Therefore, the gel ink pen refill follow-up sealant can be regarded as a 'liquid piston', and is required to be immiscible with ink and have a clear interface; no bubbles, evaporation resistance. In addition, the gel pen refill follow-up sealant also needs to have good high and low temperature stability, so that the gel pen can keep good sealing effect under the condition of large temperature change, and ink evaporation or backflow overflow is prevented; and better follow-up thixotropic fluidity, so that the sealant can follow up at any time when writing quickly, and the sealant is less stained on the pipe wall, thereby ensuring that the sealant can follow up until the ink is completely written.
The Chinese patent application CN 108690558A takes organic acid lithium salt as a thickening agent and takes synthetic oil or mineral oil as base oil to prepare the follow-up sealant. Chinese patent CN 1080750C uses dimethyl silicone oil, benzyl silicone oil and alkyl modified silicone oil as base oil, and uses polybutene and aluminum silicate as thickening agents to prepare the ink follow-up liquid for the ball-point pen. The Chinese patent CN 101280173B and the U.S. patent US 6521035B1 both use gas phase nano silicon dioxide as a thickening agent and silicon oil as base oil to prepare the follow-up sealant of the pen core of the gel pen.
The gel pen refill follow-up sealant in the prior art has the problems of poor high-low temperature performance, poor follow-up performance, poor impact resistance and the like, and the comprehensive performance is still to be improved, so that the gel pen refill follow-up sealant with excellent comprehensive performance such as high-low temperature performance, follow-up performance, impact resistance and the like is urgently needed to be provided.
Disclosure of Invention
The invention aims to provide a follow-up sealant for a gel ink pen refill, and the invention also aims to provide a preparation method and application of the follow-up sealant for the gel ink pen refill.
The main technical concept of the invention is as follows: the neutral pen refill follow-up sealant with excellent comprehensive performance generally comprises base oil and a thickening agent, and has the requirements of better viscosity, impact resistance, high and low temperature performance and follow-up property. In the development process, the invention finds that many substances have better thickening capability, but have poor follow-up property or cannot ensure better high-temperature and low-temperature performance after being compounded with base oil. Through a large number of component screening and compounding comparison experiments, the invention discovers that the gel-ink pen refill follow-up sealant with excellent comprehensive performance can be obtained by compounding the organic bentonite and the silicone oil base oil and further adding the alcohol, ketone or ester structure improving agent on the basis of the compounding of the organic bentonite and the silicone oil base oil, and simultaneously ensuring better viscosity, impact resistance and high and low temperature performance and ensuring excellent follow-up performance.
Specifically, the technical scheme of the invention is as follows:
the invention provides a follow-up sealant for a gel-ink pen refill, which comprises base oil, a thickening agent and a structure improving agent, wherein the thickening agent comprises organic bentonite, and in the follow-up sealant, the mass ratio of the organic bentonite to the base oil is 1: (18-36).
The organic bentonite is a montmorillonite-organic ammonium compound, takes bentonite as a raw material, and is prepared by intercalating an organic covering agent by using an ion exchange technology by utilizing the lamellar structure of montmorillonite in the bentonite and the characteristic that the lamellar structure can be swelled and dispersed into colloidal particles in water or an organic solvent. The organic bentonite is converted from the hydrophilic expansibility of the bentonite into the lipophilic expansibility, under the action of proper shearing force and chemical energy, the organic bentonite is dispersed in various solvents and organic media to form ultramicro or even nano sheets, and a card house type structure is formed under the action of edge hydrogen bonds, and the structure is dissociated when the external force acts, and the external force disappears or is weakened and then is recovered. In the gel-ink pen refill follow-up sealant provided by the invention, the organic bentonite and the base oil form gel, and the gel-ink pen refill follow-up sealant has good thickening property, thixotropy, high-temperature stability, chemical stability and water resistance.
The organic bentonite can be purchased from commercial sources or prepared by adopting a conventional method for preparing the organic bentonite.
The base oil is preferably silicone oil, and the kinematic viscosity of the silicone oil at 25 ℃ is 500-3000mm2/s。
The silicone oil has excellent viscosity-temperature performance and small viscosity change in a wide temperature range; the condensation point of the silicone oil is generally lower than-50 ℃, the condensation point of partial silicone oil is as high as-70 ℃, the appearance and the viscosity of an oil product are not changed after long-term storage at low temperature, and the silicone oil is base oil which can realize both high temperature and low temperature. More importantly, the thickening property of the organic bentonite can be fully exerted by compounding the silicone oil and the organic bentonite, the compound has better follow-up property, and meanwhile, the obtained follow-up agent is not easy to run off at high temperature and is not easy to condense at low temperature, and the follow-up agent has high oxidation stability, is safe, nontoxic, water-resistant and moisture-proof.
Furthermore, the invention discovers that dimethyl silicone oil, diethyl silicone oil, benzyl silicone oil and organic bentonite in methyl silicone oil are compounded according to a specific proportion, so that the viscosity, the high-low temperature performance and the follow-up property of the follow-up sealant for the refill of the gel pen can be better ensured.
The base oil is more preferably a mixture of one or more of dimethicone, diethylsilicone oil and benzyl silicone oil. In the follow-up sealant, the mass ratio of the organic bentonite to the base oil is 1: (23-33).
The structure improving agent is preferably one or a mixture of methanol, ethanol, acetone and propylene carbonate.
The invention preferably adopts the organic bentonite with the passing rate of not less than 98 percent under the condition of 75 mu m dry sieve.
Specifically, the follow-up sealant is prepared from the following raw materials in parts by weight: 90-97 parts of base oil; 2-10 parts of a thickening agent; 0.5-5 parts of structure improving agent.
Through compounding and screening of all components, the optimal combination mode is determined, namely benzyl silicone oil (base oil), organic bentonite (thickening agent) and propylene carbonate (structure improver) are compounded according to a specific proportion, and the obtained follow-up sealant has better high and low temperature performance, follow-up property and impact resistance. As a preferable scheme of the invention, the preparation raw material of each 100 parts of the follow-up sealant comprises the following components in parts by weight:
90-97 parts of benzyl silicone oil;
2-5 parts of organic bentonite;
0.5-2 parts of propylene carbonate.
The invention further provides a preparation method of the follow-up sealant, so that the performances of all components in the formula can be well exerted.
The invention provides a preparation method of a follow-up sealant, which specifically comprises the following steps:
(1) mixing base oil accounting for 50-70% of the total mass of the base oil with organic bentonite, and heating to 50-60 ℃;
(2) adding a structure improving agent, and continuously stirring for 0.5-1.5h to ensure that the organic bentonite is fully expanded and activated in the base oil;
(3) heating to 90-100 deg.C, stirring for 0.3-1h, refining, and removing excessive structure improving agent;
(4) and after refining, adding the rest base oil, rolling, degassing and filtering.
The invention provides the use of the follower sealant in the manufacture of a gel-ink pen refill or gel-ink pen.
The invention provides a gel pen refill which contains the following sealant.
The invention provides a gel pen containing the follow-up sealant.
The invention has the beneficial effects that: the gel ink pen refill follow-up sealant provided by the invention is mutually incompatible with ink, has excellent viscosity, impact resistance, high and low temperature performance and follow-up property and excellent comprehensive performance, can be used for gel ink pen refills, and plays roles of sealing and liquid piston. The assembled neutral pen core has good sealing performance and impact resistance, can keep the performance of the neutral pen core under the conditions of high temperature and low temperature, and meanwhile, in the writing process, the sealant can move along with the reduction of the printing ink, so that the printing ink can be prevented from evaporating, and the printing ink can be smoothly written.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The experimental procedures used in the following examples are conventional unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified, wherein the organobentonite is obtained from Zhejiang Fenghong New materials Co., Ltd, has a volatile content (105 ℃ C., 2 hours) of not more than 3.5%,specific gravity of 1.7g/cm2And the passing rate of a 75-micron dry sieve is not less than 98 percent. Dimethicone, Dimethicone and Benzylsicone were purchased from Anhui Aiyuta Silicone Ltd and had kinematic viscosities at 25 ℃ of 2000mm, respectively2/s，2500mm2S and 2000mm2/s。
Example 1
The embodiment provides a follow-up sealant for a gel ink pen refill, which is prepared by the following method:
firstly, 513g of simethicone and 32g of organobentonite are added into a reaction kettle, the materials are fully mixed and stirred, the temperature is heated to 50 ℃, 8g of ethanol is added, and the stirring is continued for 1 hour, so that the organobentonite is fully expanded and activated in the base oil. Heating to 90 deg.C, stirring for 0.5h, and removing excessive ethanol in the system. And after refining, adding the rest 257g of dimethyl silicone oil, rolling for three times by a three-roll mill, and degassing and filtering to obtain the gel pen refill follow-up sealant.
Example 2
The embodiment provides a follow-up sealant for a gel ink pen refill, which is prepared by the following method:
firstly, 576g of simethicone and 36g of organobentonite are added into a reaction kettle, the mixture is fully mixed and stirred, the temperature is heated to 50 ℃, 8g of acetone is added, and the stirring is continued for 1 hour. The temperature is raised to 90 ℃, and the mixture is stirred for 0.5h, so that the excessive acetone in the system is removed. And after refining, adding the rest 288g of dimethyl silicone oil, rolling for three times by a three-roll machine, and degassing and filtering to obtain the gel pen refill follow-up sealant.
Example 3
The embodiment provides a follow-up sealant for a gel ink pen refill, which is prepared by the following method:
firstly, 515g of diethyl silicone oil and 28g of organic bentonite are added into a reaction kettle, fully mixed and stirred, heated to 50 ℃, added with 8g of propylene carbonate and continuously stirred for 1 hour. Heating to 90 ℃, stirring for 0.5h, and removing the redundant propylene carbonate in the system. And after refining, adding the rest 257g of dimethyl silicone oil, rolling for three times by a three-roll mill, and degassing and filtering to obtain the gel pen refill follow-up sealant.
Example 4
The embodiment provides a follow-up sealant for a gel ink pen refill, which is prepared by the following method:
firstly, 517g of benzyl silicone oil and 28g of organobentonite are added into a reaction kettle, the materials are fully mixed and stirred, the temperature is heated to 50 ℃, 8g of acetone is added, and the stirring is continued for 1 hour. The temperature is raised to 90 ℃, and the mixture is stirred for 0.5h, so that the excessive acetone in the system is removed. And after the refining is finished, adding the remaining 259g of dimethyl silicone oil, rolling for three times by a three-roll mill, and degassing and filtering to obtain the gel pen refill follow-up sealant.
Example 5
The embodiment provides a follow-up sealant for a gel ink pen refill, which is prepared by the following method:
firstly, 453g of benzyl silicone oil and 21g of organic bentonite are added into a reaction kettle, fully mixed and stirred, heated to 50 ℃, added with 8g of propylene carbonate and continuously stirred for 1 hour. Heating to 90 ℃, stirring for 0.5h, and removing the redundant propylene carbonate in the system. And after refining, adding the rest 226g of benzyl silicone oil, rolling for three times by using a three-roll mill, and degassing and filtering to obtain the gel pen refill follow-up sealant.
Comparative example 1
The preparation method of the follow-up sealant for the gel-ink pen refill of the comparative example is the same as that of example 5, and the difference is that the thickening agent, namely the organic bentonite, is replaced by the silicon dioxide (the specific surface area is 150 m)2/g)。
Comparative example 2
The following sealant for a pen core of a gel-ink pen of this comparative example was prepared in the same manner as in example 5 except that no structure improver was added during the preparation.
Comparative example 3
The preparation method of the following sealant for the pen core of the gel-ink pen in the comparative example is the same as that in example 5, except that the base oil benzyl silicone oil is replaced by poly-alpha-olefin (kinematic viscosity at 40 ℃ is 1300 mm)2In s). Examples of the experiments
The performance test of the gel pen refill following sealant in each of the above examples and comparative examples was carried out, and the performance test method and evaluation criteria were as follows:
1. cone penetration test:
the standard cone is free to fall to penetrate the sample filled in the standard fat cup to a depth of 0.1mm over 5 seconds. Reference is made to the standard GB/T269-1991.
2. And (3) drop point testing:
the temperature of the first sample dropped from the sample in the cup of the droppoint meter is the dropping point of the sample in units of ℃. Reference is made to the standard GB/T4929.
3. Low temperature similar viscosity test:
low temperature flow properties in Pa · S for apparent samples. Reference is made to the standard SH/T0048.
4. Follow-up test:
the gel ink was drawn at a drawing speed of 20 to 25mm/s, and the state of remaining sealant was observed and evaluated according to the following criteria:
the remaining amount of sealant did not change significantly: a. the
A small reduction in the remaining amount of sealant occurred: b is
The residual quantity of the sealant is obviously reduced, and the wall sticking phenomenon is obvious: c
5. And (3) testing the falling resistance:
find a long tubule of 1m, the bottom pad china fir plank, the tubule is vertical places, assembles the sealant to the gel ink refill in, with the sealant one end of refill down, nib one end up, makes its free fall whereabouts from the upper end of tubule, and every sample is done 3 times, observes the sealant state and evaluates according to following standard:
no change: a. the
A small amount of sealant runs off from the tail of the refill, and a small amount of ink is mixed into the sealant: b is
The interface of the sealant and the ink is disordered, and a large amount of sealant is lost from the tail part of the pen core: c
6. High temperature drip performance test:
the sealant-fitted gel ink cartridge was vertically inverted for 30 days at a temperature of 50 ℃ and a humidity of 60%, and the degree of dripping of the sealant to the inner wall of the barrel was observed and evaluated according to the following criteria:
no dripping: a. the
The sealant has a portion that drips to the inside wall of the barrel: b is
The sealant trickles down the inside wall of the barrel in bulk and there is a portion that flows out of the barrel: c
7. And (3) testing low-temperature fluency:
the paper was quickly scored at 0 ℃ and the line breaks or hollowness observed and tested according to the following criteria:
line interruption and no interruption: a. the
Few broken lines or hollows: b is
Severe line breakage or hollowing: C.
specific test items and test results are shown in tables 1 and 2.
TABLE 1 test for Performance of follow-up sealants for gel ink pens cartridges (1)
TABLE 2 test for Performance of follow-up sealants for gel ink pens cartridges (2)
As can be seen from tables 1 and 2:
in comparative example 1, the addition of silica increases the system consistency and viscosity to a greater extent, resulting in poor follow-up and low temperature fluidity.
In comparative example 2, no structure-improving agent was added, sufficient hydrogen bonds were not generated in the system, only weak gel was formed, the consistency of the whole system was low, and various performances were poor.
In comparative example 3, the high and low temperature properties of the substituted polyalphaolefin were inferior to those of the silicone oil, and the high temperature dripping property and the low temperature flow property thereof were inferior.
Compared with the gel ink pen refill follow-up sealing agent in the comparative example, the gel ink pen refill follow-up sealing agents in the examples 1-5 are better in follow-up property, falling resistance, high-temperature dripping property and low-temperature fluency, and the gel ink pen refill follow-up sealing agent in the example 5 is optimal in comprehensive performance.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The gel pen refill follow-up sealant is characterized by comprising base oil, a thickening agent and a structure improving agent, wherein the thickening agent comprises organic bentonite, and the mass ratio of the organic bentonite to the base oil in the follow-up sealant is 1: (18-36).
2. The follower sealant according to claim 1, wherein the base oil is a silicone oil having a kinematic viscosity at 25 ℃ of 500 to 3000mm2/s。
3. The follower sealant according to claim 2, wherein the base oil is a mixture of one or more of dimethicone, diethylsilicone oil, and phenylmethylsilicone oil; in the follow-up sealant, the mass ratio of the organic bentonite to the base oil is 1: (23-33).
4. A follower sealant according to any of claims 1 to 3, wherein the structure improver is a mixture of one or more of methanol, ethanol, acetone and propylene carbonate.
5. A follower sealant according to any of claims 1 to 4, wherein the organobentonite has a 75 μm dry sieve passage of not less than 98%.
6. The follow-up sealing agent according to any one of claims 1 to 5, wherein the follow-up sealing agent is prepared from the following raw materials in parts by weight: 90-97 parts of base oil; 2-10 parts of a thickening agent; 0.5-5 parts of structure improving agent.
7. A method for preparing a follow-up sealant according to any one of claims 1 to 6, comprising the steps of:
(1) mixing base oil accounting for 50-70% of the total mass of the base oil with organic bentonite, and heating to 50-60 ℃;
(2) adding a structure improving agent, and continuously stirring for 0.5-1.5h to ensure that the organic bentonite is fully expanded and activated in the base oil;
(3) heating to 90-100 deg.C, stirring for 0.3-1h, refining, and removing excessive structure improving agent;
(4) and after refining, adding the rest base oil, rolling, degassing and filtering.
8. Use of the follower sealant according to any one of claims 1 to 6 in the manufacture of a gel-ink pen cartridge or gel-ink pen.
9. A refill for a gel ink pen, which comprises the follow-up sealing agent according to any one of claims 1 to 6.
10. A gel-ink pen comprising the follower sealing agent according to any one of claims 1 to 6.
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| CN202010570552.1A CN111909756A (en) | 2020-06-19 | 2020-06-19 | Gel ink pen refill follow-up sealant and preparation method and application thereof |
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| CN202010570552.1A CN111909756A (en) | 2020-06-19 | 2020-06-19 | Gel ink pen refill follow-up sealant and preparation method and application thereof |
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Cited By (1)
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| CN114989782A (en) * | 2022-07-14 | 2022-09-02 | 丰城三友制笔科技有限公司 | Ink follow-up agent for emulsified oil and preparation method and application thereof |
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| CN114989782A (en) * | 2022-07-14 | 2022-09-02 | 丰城三友制笔科技有限公司 | Ink follow-up agent for emulsified oil and preparation method and application thereof |
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Application publication date: 20201110 |