JPS61501573A - Durably dusting-free pigment and dye products and methods for their production and instruments therefor - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] For pigments and paints, dust and dust must be used so as not to cause dust-like emissions during processing. There are increasing attempts to create ting-free formulations. This kind of formulation without dusting is particularly desired to avoid color contamination during handling of various products, and It also enables accurate dosing. Besides avoiding dusting losses, these formulations Cleaner and safer work eliminates the health risks of working with toxic pigments and dyes. lower.

The safest route is through paste products, where surface-active substances and solvents such as Additives are added in amounts sufficient to reach a dusting-free paste state. this These pastes contain dispersion media, anti-sedimentation agents and coloring agents as required for the specific application. Medications such as drugs are also often added. The pigment concentration in these pastes is Depending on the fineness and structure of each pigment and the amount of vehicle required, the number of It can be between 0'X and 90%. In the production of pigment pastes, dry pigments are Starting from this, mix it with each component.

The disadvantage of pigment paste is that it requires careful cleaning of the packaging container for dispensing. This is often seen.

The purpose of this invention is to enable easy dispensing and measuring because it flows smoothly. We aim to create dusting-free pigment and dye products that maintain their properties for a long time. be.

There are already many known methods. According to Dle-OS 2723921, Combinations of esters of 7-talic acid and ter-7-talic acid with esters of fatty acids and surface-active substances Metallic acid is added to an aqueous pigment suspension and dried after P filtration. Salt dusting tendency is suppressed. This type of product exhibits less dusting. However, it does not mean that there is no dusting in terms of durability. Thus, Example 1 of this patent application Products made in accordance with the dusting test using the Hoibatsuha Dusting Measuring Instrument The value was 8397100f. DB shows other methods and means. OS 2931771, D'IA- OS2523096, US-P8 3560134, EU-08 0056160 and DE-OS It is 2841566.

The object of this invention is a durable non-dusting pigment/dye product, which is 7 In addition to 5 to 97.5% of pigments, an amount of 0.5 to 10% of surface-active substances and strong Moisturizes a dry homogeneous mixture of pigments or dyes and surface-active substances during shear stress. Medicine for smooth spots+! Contains F12-25% and is at the lubrication point as defined. surface The active substance may be a suitable substance for the respective pigment or dye type and its subsequent use. All surface-active agents, ionic or non-ionic, commercially available You can use it. But particularly preferred are long-chain polymers of the type ``effective dispersant.'' esters, especially those with at least four carbon atoms between the hydroxyl and carboxylic acid groups. a saturated or from unsaturated aliphatic W-hydroxycarboxylic acids or from such hydroxycarboxylic acids. carboxylic acids and carboxylic acids without hydroxyl groups, especially those with up to 20 C atoms It is a polyester derived from a mixture of

These suitable esters include those described in D'E-OS 2162484. (It also includes Terugiri Esther), and I will quote it here.

It is important that the surface-active substance is not applied over the dry pigment. or the pigment is not already dry once, but is still wet from production. The process involves treating pigments with surface-active substances. Otherwise, the surface properties of the No. Therefore, it is appropriate to mix this agent with the pigment mud and then dry it. That's true.

The concept of pigment also includes dyes.

The resulting dry mixture of pigments and surface-active substances is then mixed with strong shear stress. All substances that produce the effect of and can be used as substances that lead to the lubrication point. can be used in areas of use such as paints, racks, printing inks and plastics. The technical requirements for the application of dark staining can be taken into account. Water, organic solvent, softening, For example, there are substances that become liquid when exposed to high temperatures, such as wax. child Suitable here are drugs that do not vaporize at all or to any extent. Usually for economic reasons Mineral oil is preferred. This is because the results are excellent and the price is reasonable.

Mineral oils are considered to be aliphatic oils that are readily liquid at room temperature and have a boiling point above 70°C. , alicyclic and/or aromatic hydrocarbons. Preferred in some cases fats which may contain different amounts of cycloaliphatic and/or aromatic hydrocarbons. It is an aliphatic hydrocarbon. It is therefore an industry consisting of petroleum refined in various ways. mineral oils as well as synthetic hydrocarbons, such as Fischer tortoises with a specified boiling range. Also includes Ropsch mixtures. It can therefore be of any origin, e.g. petroleum , tar or its distillation products or carbonization, consisting mainly of hydrocarbons. Contains all saponifiable substances.

Particularly preferred are synthetic isoparaffins. However, water is also suitable, and a little If the amount of surfactant is 10 to 15 times water. Products made dust free with water If necessary, the final product should be packaged watertight or airtight to prevent water from escaping. should be equipped.

These durable dusting-free pigment products are made as follows. pigment An appropriate amount of 0.5 to 10% by weight based on the total weight of the final product is added to the slurry. If the combination of pigment and surface-active substance is added after homogeneous distribution, In some cases, it is isolated as a presscake and then dried, and then the dried product is Agents that bring the mixture to the point of lubrication under the action of strong shear forces, especially 70 to 360 ℃, preferably 180 to 280℃, specifically boiling range of 180 to 250℃ After mixing with the surrounding mineral oil while applying strong shear stress until the lubrication point is reached, Regranulation is performed in a manner known per se.

When using water as a means to reach the lubrication point, water can be added later. Combination of pigments or dyes and surfactants, which can also be present as cakes or press cakes. 2 to 25%, especially 10 to 1, since the mixture is only partially dried. 5% residual moisture remains and the resulting moist mixture becomes moist under shear stress. It is brought to the slipping point and regranulated in some cases. At that time, this moisture Apart from slight changes during subsequent processing, it is also present in the final product.

Homogeneous distribution of the surface-active substances in the pigment slurry is achieved by thorough mixing in known manner. Therefore, it is done. Isolation as a press cake can be carried out using suitable filtration equipment, e.g. This is done using filter presses, drum filters, suction funnels, etc. press cake or equivalent material that can be supplied by a technically effective drying method; Produces dehydrated products.

Treatment with chemicals that lead to lubrication points can be done using, for example, kneading machines, high-power mixers, or shovel mixers. This is done in mixing equipment such as This creates shear stress and the product reaches the lubrication point after about 2 hours of processing at most. 15 The degree of shear stress is such that the lubrication point is reached within minutes to 45 minutes, especially about half an hour. Liked. The product is usually free-flowing and fine-grained with virtually no dusting. occurs.

A sticky putty-like paste is still forming at the lubrication point in this patent application. By determining the oil coefficient according to DIN 53199 ( (see also Ullmann Encyclopedia of Industrial Chemistry, 4th edition, volume 18, page 565) That's exactly what it says. The specified lubrication point within the meaning of this patent application is reached by the dust There is no drying of the above, which leads to a slight lubrication effect on the walls of the mixing device. This is when fine grains are formed. Therefore, the powder required to reach this lubrication point The amount of dust binder, e.g. oil, for the determination of the oil coefficient according to DIN 53199 The amount of oil required is less.

By adding surface-active substances to the pigment before drying, optimum wetting is achieved and This can be achieved by adding, for example, mineral oil to the dry product of pigments and surface-active substances. Mineral oil makes it possible to obtain pigment preparations that are absolutely dusting-free. Required only in relatively small proportions. Equal amount of surface-active substance in pre-dried product When adding mineral oil, add approximately twice the amount to similarly eliminate dusting. Mineral oil, for example, 20% or more is required to replace IOX according to the method of the present invention. .

This method is used in principle to remove all pigments that occur in wet conditions and are separated as todoro. It can be applied to dyes. It is also used for example in lead chromate, lead molybdate, Inorganic and organic pigments and dyes such as zinc chloride, nickel titanium yellow, chromium Mixed phase pigments such as titanium yellow, 7-tawacyanine, anthraquinone, azo pigments, Lacnis azo pigment, disazo condensation pigment, isoindoline, indigoid dye , quinacridone, perylene, etc.

The pigment or dye mud and surfactant mixture, which usually contains about 50% water, is thoroughly After homogenization, it can be sent directly to drying, or if you want to reduce the moisture content, use a suitable method. It is further dehydrated in a press, for example a high-pressure press, and then sent for drying. Do that This will save on drying costs. Drying of this mixture is usually carried out, for example on a belt or At ambient temperature of 120-130℃ on a rotary grinder or normally Zoo-120℃ This can be done in a vacuum dryer using a temperature of . Since the mixture contains organic matter, Ensure that the drying conditions, especially the temperature, do not damage the material, e.g. avoid localized overheating. You should be careful.

Dusting characteristics can be measured using a Heubatsuha dusting measuring instrument as shown in the attached diagram. I did it.

This dusting meter detects dusting tendencies of powdery and granular materials as accurately as possible. Developed for accurate analysis. Quantitative data on dusting properties are available from chemical techniques. This is because it is important for surgical and operational safety. Conventionally, dusting tendency was evaluated. The value may be determined by analogy with the proportion of fines present in the material or by estimation. (However, this type of method can make big mistakes.

This is because dust particles are often formed only by movement or wear and tear). Here, the tendency of dusting in material handling can be seen in a more realistic manner. Besides that The test material is interlocked during all measurements. Dust generation of powder or granular material with a volume of λ5t Move it at 30 revolutions per minute for 5 minutes in the raw container No.2. The attached baffle plate is in the feeding process. during which dust is captured from the air stream and removed from the dust generating container. It is transported and separated on a filter with limited porosity. Coarse particles are coarse 91 is held in the separator 3. Air is sucked by vacuum pump j, It is recorded and emitted by an air tank with flow meter 6.

A motor/drives the device.

A ray of light that passes through a receiving container when dye dust is stirred up and lowered once inside the container. Compared to dusting meters, which measure dust values by weakening the , has the advantage of being able to closely measure the conditions that appear during the mixing and injection process. Motsu.

Constant amount 100 f Measurement time: 5 minutes Rotation: 30 per minute Air flow rate 0.25- Dust generating container 15 The following examples illustrate this invention and are considered herein as dusting-free preparations. The maximum value is O or 5M9/100 measured with a Heubach Tasting meter. A dust value of f is generated.

Example 1 Polyester-based surface active substance 15 in 50% chromate pigment mud of 1 Kp and mixed well with a stirrer. Knead machine or shovel into pigment after drying Add the ION mineral oil in the mixer and mix on high intensity until an even distribution of additives is achieved. continued. It can be distinguished by the appearance of smooth, non-dusting fine grains. By life.

This usually takes 30 minutes. Hoipatsuha dusting of the processed finished product When subjected to dusting measurement with a measuring device, the pigment 100 became the value of the bow. Ta. The untreated dry pigment sample had a dusting value of 90'Iv/oof. Added 10f of a surface-active substance based on 50% zinc chromate nigiri ester of Kf. Well, mix well while stirring.

After drying, add 13% mineral oil to the pigment in a kneader or shovel mixer. The mixture was exposed to the pulsating action of the mixing device until it was completely homogeneously distributed. After about 30 minutes Free-flowing fine grains with no dusting are produced, and the dusting value is It was measured with a dusting meter and was equal to 0.

Dusting value for untreated dry zinc chromate sample is 25011+9/10 It became 0t.

Example 3 7 Talocyanine blue press cake (approx. 36% solids) 300fK isopropate 150t, aminomethyl propatool 5.5t and polyester based surface active substances &2? Add the mixture of 100? After adding water, stir in a dissolver. did. The pigment mud prepared in this way was dried in a dryer, and an intermediate powder was produced in an experimental grinder. Add 20% mineral oil (based on solids) in a mixing device after crushing to ensure even distribution of additives Mixing intensity was continued until . Smooth without dusting after 20-30 minutes The dusting value was measured using a Heubach dusting meter. When I looked at it, it was equal to 5wV'Zoo f. The unprepared 7-talocyanine pigment is It has a dusting value of 2500 to 3soo IR9/100t.

Example 4 1568 F anthraquinone pigment mud (solid matter approx. 28X) with aminomethyl propane adding a mixture of tool 239 and polyester-based surface active material 252; Stir in the dissolver for about 30 minutes. Antifoaming agent 7.51 was also added to prevent foaming. Ta. The mud thus prepared was dried in a dryer and then pre-ground in a laboratory grinder. Ta.

This preparation was placed in a mixer and 20X mineral oil was added and mixing continued for approximately 30 minutes.

Afterwards, a free-flowing, non-dusting fine grain appears, and its dusting value is When measured with a Bach dusting meter, it was less than 5 cm per 100 f of pigment. drying The unprepared anthraquinone pigment was 3500 to 4500 μ/10 It has an extremely high dusting value.

Polyester-based surface-active substances 11 to 50% chloride pigment mud of 1 to 1 and mixed well with a stirrer. After drying, put the pigment in a heated kneading machine for 15 minutes. Added X molten wax and continued vigorous mixing until even distribution of additives was achieved. . This can be recognized by the appearance of free, dusting-free granules. It is. This usually takes about 30 minutes. The pigment should be heated above the melting point of the wax beforehand. temperature. The melting point of the wax used was 79°C.

The dusting measurement of the preparation thus made is 5M9/1o.

It was t. A Heubach dusting measuring instrument was used for measurement.

Of course, products according to this invention may contain pre-dispersion or anti-friction additives as required for their particular use. Adjunctive agents such as these can also be added. This addition is a drug that creates lubrication points @b) It is appropriate to carry out this process together with the addition of . Similarly, as shown in the example, Adding auxiliary agents for mixing or kneading, such as antifoaming agents, at each step You can also do that.

In the case of all these adjunct drugs, amounts common and well known in the art are used. , also for each special case by a small number of preliminary tests, i.e. surface activity Check the amount depending on the amount and type of agent and the amount and type of agent that causes lubrication points. Can be done.

Desirable embodiments of this invention include the following.

Additives include additives that are liquid in the product or that become liquid when the temperature exceeds 50°C. There is. As a liquid additive, it is desirable that the boiling range of water is up to 360℃. Mineral oil at 180-280°C may be preferable, while additives that are liquid at high temperatures are preferred. has a melting point of 50-200°C. The substances that lead to the lubrication point are 25% by weight or resulting in a content of 2 to 25% by weight in the final product (air (if oxidation occurs). In the case of mineral oils, the addition is preferably 5. 15%, especially 10%. Additives that become liquid at temperatures exceeding 50℃ are particularly It may be a wax or paraffin material. Pigments homogenized with surface-active substances or dye furnace sludge, in suitable applications such as filter presses, suction funnels, drum filters, etc. It is isolated as a presscake using appropriate filtration equipment.

Importantly, the still wet pigment is treated with the surfactant; Pigments can only be dehydrated mechanically, e.g. by pressing or centrifuging; Although a slight drying effect may occur, for example from air or hot air drying, the overall condition is still damp. , so the surfaces of the pigment particles are not yet dry and the humidity on these surfaces Even though the humidity in the mud press cake has dropped, it is still damp.

The concept of pigments here also includes dyes.

rlsw--Amm1mm PCT/EP 84100380INTERNAT IONAL APPLICAτrON No, PCT/EP 8410031 110 (SA 85241US-A-349931510103/70 No. Continuation of page 1 Priority Claim Section 0198 December 2nd [Sat] West Germany (DE) [Yes] P 3343 742.4 [phase] 198 j December 8 [phase] West Germany (DE) [stock] P334 4464.1 [Phase] 198th December 8th [Phase] West Germany (DE) ■P334 4463.3■ Initiator Adrian, Gerhard Federal Republic of Germany'y I! f table Showa 61-501573 (7) 3380 Goslar 1 Tarshtra Tsuse 20a

Claims (10)

[Claims] 1. As a dust remover a) a surfactant in an amount of 0.5-10% and b) a dry mixture of pigment and surfactant After mixing the material (facial (depending on the fineness, morphology and subsequent intended use of the dye or dye product) 2 to 2 Permanently non-dusting pigments containing in an amount of 5% and the remainder consisting of pigments or dyes ・It is a dye product, and depending on the type of pigment or dye, Add an appropriate surface-active substance or mixture thereof depending on the purpose of use, and mix until homogeneous. The pigment and surfactant combination may be prepared after distribution, sometimes as a breath cake. After isolation, dry the dried product and lubricate the mixture under strong shear stress. Adding liquid, flowable or hot liquid agents and applying strong shear stress leading to mixing until a lubrication point is reached and then optionally mixing in a manner known per se. The product characterized in that it is obtained by regranulation. 2. The surfactant is a long chain polyester of the type "effective dispersant", it is Carboxy with at least four carbon atoms between the hydroxyl group and the carboxylic acid group a saturated or unsaturated aliphatic w- having a total of at least nine carbon atoms including the radicals; From hydroxycarboxylic acid or with this kind of hydroxycarboxylic acid and hydroxy group as claimed in claim 1, characterized in that it is derived from a mixture with a carboxylic acid free of Products according to section 1. 3. Water, mineral oil or a hot liquid substance (pigment (depending on the fineness, morphology and subsequent intended use of the dye product) 2 to 25 Product according to claim 1 or 2, characterized in that it contains in an amount of %. 4. Said claim characterized in that there is an amount of water in the final product of 10 to 15%. Products according to one of the items 1 to 3 of the scope. 5. Depending on the type of pigment or dye and the purpose of each use, Add a suitable surface-active substance or mixture thereof depending on the purpose, and after homogeneous distribution add the pigment. and surfactant combination, sometimes dried after isolation as a breath cake. and then the dried product is injected with a liquid that brings the mixture to the point of lubrication under strong shear stress. Add a liquid, fluid, or hot liquid agent and moisturize while applying strong shear stress. Mix until the slip point is reached and then optionally regranulate in a manner known per se. Claims 1 to 3 are characterized by the addition of a surfactant and an additive. Process for manufacturing pigment and dye products according to paragraph 4. 6. The above claim, characterized in that wet taro mud of pigments or dyes is used as raw material. Method according to scope item 5. 7. Amounts of surface-active substances of 0.5 to 10%, preferably 1 to 5%, especially 3% 7. A method according to claim 5 or 6, characterized in that it is used in. 8. Liquid with a melting point of 50 to 200℃ or at 50℃ as a substance that leads to the lubrication point , especially wax or varaffin substances that become liquid at 50 to 200°C. Claim 5, characterized in that it is used in an amount of 25%, preferably 15%. A method according to one of paragraph 7. 9. Applying liquid or heat-liquefied additives to dry products containing surface-active substances Add additives and use a suitable mixer, such as a high-power mixer, kneader, or shovel mixer. Claim 1, characterized in that the mixture is mixed in a mixer until a lubrication point is reached. Method according to one of paragraphs 5 to 8. 10. The built-in baffle plate is rotated by the prime mover and simulates feeding. A dust generating container 2 containing a dust generating container 2 and a fin having limited porosity carried out from the dust generating container 2. a pump 5 for generating air flow to capture the dust separated by the filter 4; There, a coarse filter is used to retain coarse particles between the filter 4 and the dust generating container 2. A separator 3 is placed and also measures the air flow rate from which the air is released. Particularly in conditions close to reality, characterized by a total of six airlocks. For measuring the dusting properties of pigment or dye products according to paragraphs 1 to 4 equipment.