JP2023164367A - Method for producing colorful black lacquer - Google Patents

Method for producing colorful black lacquer Download PDF

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JP2023164367A
JP2023164367A JP2023073090A JP2023073090A JP2023164367A JP 2023164367 A JP2023164367 A JP 2023164367A JP 2023073090 A JP2023073090 A JP 2023073090A JP 2023073090 A JP2023073090 A JP 2023073090A JP 2023164367 A JP2023164367 A JP 2023164367A
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lacquer
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vacuum distillation
kurome
raw lacquer
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秀悟 及川
Shugo Oikawa
福律 李
Bok-Luel Lee
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Abstract

To provide a method that can efficiently produce colorful black lacquer.SOLUTION: A method for producing colorful black lacquer includes a step for subjecting raw lacquer liquid to vacuum distillation, wherein a colorant is added to the raw lacquer liquid, or added to transparent black lacquer obtained after the vacuum distillation. Preferably, the vacuum distillation should be performed under these conditions: it should continue until the treated black lacquer has a moisture content of 3 wt.% or less; the pressure should be lowered by 25-60 hPa below the vapor pressure of the raw lacquer liquid; the process should last for at least 30 minutes; and it should be conducted at a temperature range of 20-35°C. The colorant preferably should be an inorganic pigment or an organic pigment, more preferably iron oxide, mercury sulfide, or a lake pigment.SELECTED DRAWING: None

Description

本発明は、カラフル黒目漆の製造方法に関する。 The present invention relates to a method for producing colorful Kurome lacquer.

漆は、古来より用いられてきた天然塗料である。一般の有機塗料は、塗膜の乾燥反応により皮膜が形成されるのに対し、漆の皮膜形成には、その成分であるラッカーゼ及びウルシオールが関与する。すなわち、漆を木材等の基材に塗布すると、ラッカーゼが空気中の酸素を用いてウルシオールの酸化反応を生じさせ、更に、水分の存在下でウルシオールを重合(架橋:polymerization)して基材上に黒色のフィルムを形成する(非特許文献1)。この点で、漆は一般の有機塗料と異なる、いわゆる生体塗料と言える。
漆産業では、カラフル黒目漆が国内外から着目されている。現在のカラフル黒目漆の製造プロセスは生漆を加熱撹拌し精製して得られる透黒目漆に色素を添加混合する方法により行われている。水分含有量が低い透黒目漆に大量の顔料を加えると粘度が急激に増加するため、カラフル黒目漆の生産は透黒目漆の生産と比較してより困難とされている。
Lacquer is a natural paint that has been used since ancient times. In general organic paints, a film is formed by a drying reaction of the paint film, whereas the film formation of lacquer involves its components, laccase and urushiol. That is, when lacquer is applied to a base material such as wood, laccase causes an oxidation reaction of urushiol using oxygen in the air, and further polymerizes urushiol in the presence of moisture to form a base material. A black film is formed on the material (Non-Patent Document 1). In this respect, lacquer can be said to be a so-called biological paint, different from general organic paints.
In the lacquer industry, colorful black-eyed lacquer is attracting attention both domestically and internationally. The current manufacturing process for colorful Kurome lacquer is carried out by adding and mixing pigments to transparent Kurome lacquer obtained by heating, stirring and refining raw lacquer. The production of colorful Kurome lacquer is said to be more difficult than the production of Transparent Kurome lacquer, as the viscosity increases rapidly when a large amount of pigment is added to Kurome lacquer, which has a low water content.

熊野谷 従(1991年)Jasco Report、33巻、2号、15-29ページKumanoya, T. (1991) Jasco Report, Vol. 33, No. 2, pp. 15-29.

透黒目漆の調製の際には、その水分量を調整して行うところ、従来の方法のように透黒目漆に色素を混合すると、上述のとおり粘度が上昇し、水分量が変化するため、色素を均一に混合して水分量を3重量%以下となるまで蒸発させることは非常に手間がかかる。そのため、カラフル黒目漆の生産はコストが高いという問題がある。一方、原料生漆の加熱撹拌前に色素を添加すると、添加後に系内の粘度が上昇し、加熱撹拌による水分蒸発に長時間を要し、作業が非常に困難となることが予想される。 When preparing transparent Kurome lacquer, the water content is adjusted. However, when pigments are mixed into Transparent Kurome lacquer as in the conventional method, the viscosity increases as mentioned above and the water content changes. It is very time consuming to uniformly mix the pigments and evaporate them until the water content is 3% by weight or less. Therefore, there is a problem in that the production cost of colorful Kurome lacquer is high. On the other hand, if pigments are added before heating and stirring the raw raw lacquer, the viscosity within the system will increase after the addition, and it is expected that it will take a long time to evaporate water by heating and stirring, making the work extremely difficult.

本発明は、カラフル黒目漆を効率的に製造できる方法を提供することを目的とする。 An object of the present invention is to provide a method that can efficiently produce colorful Kurome lacquer.

本発明は、〔1〕~〔9〕を提供する。
〔1〕生漆を含む原料生漆液を減圧蒸留する工程を含み、着色剤を原料生漆液に添加するか、又は、減圧蒸留後に得られる透黒目漆に添加する、カラフル黒目漆の製造方法。
〔2〕減圧蒸留は、処理後の水分量が3重量%以下となるまで行う、〔1〕に記載の製造方法。
〔3〕減圧蒸留は、原料生漆液の蒸気圧より25~60hPa減圧して行う、〔1〕又は〔2〕に記載の製造方法。
〔4〕減圧蒸留は、30分以上行う、〔1〕~〔3〕のいずれか1項に記載の製造方法。
〔5〕減圧蒸留は、20~35℃で行う、〔1〕~〔4〕のいずれか1項に記載の製造方法。
〔6〕着色剤は、無機顔料又は合成顔料である、〔1〕~〔5〕のいずれか1項に記載の製造方法。
〔7〕着色剤は、酸化鉄、硫化水銀、レーキ顔料である、〔1〕~〔6〕のいずれか1項に記載の製造方法。
〔8〕原料生漆液又は生漆を、35℃以下で常圧下撹拌又は磨砕するなやし処理工程、及び/又は、ろ過処理工程を更に含む、〔1〕~〔7〕のいずれか1項に記載の製造方法。
〔9〕なやし処理工程は、密閉容器へ格納し容器ごと撹拌する方法、乳鉢と乳棒を用いて粉砕する方法、及び擂潰機を用いて撹拌及び粉砕する方法の少なくともいずれかによって行う、〔8〕に記載の方法。
The present invention provides [1] to [9].
[1] A method for producing colorful Kurome lacquer, which includes a step of distilling raw raw lacquer containing raw lacquer under reduced pressure, and adding a coloring agent to the raw raw lacquer or to transparent Kurome lacquer obtained after vacuum distillation.
[2] The production method according to [1], wherein the vacuum distillation is performed until the water content after treatment becomes 3% by weight or less.
[3] The production method according to [1] or [2], wherein the vacuum distillation is performed by reducing the pressure by 25 to 60 hPa from the vapor pressure of the raw raw lacquer solution.
[4] The production method according to any one of [1] to [3], wherein the vacuum distillation is performed for 30 minutes or more.
[5] The production method according to any one of [1] to [4], wherein the vacuum distillation is carried out at 20 to 35°C.
[6] The manufacturing method according to any one of [1] to [5], wherein the colorant is an inorganic pigment or a synthetic pigment.
[7] The manufacturing method according to any one of [1] to [6], wherein the colorant is iron oxide, mercury sulfide, or lake pigment.
[8] Any one of [1] to [7], further comprising a soothing treatment step of stirring or grinding the raw raw lacquer liquid or raw lacquer under normal pressure at 35°C or lower, and/or a filtration treatment step. The manufacturing method described in.
[9] The coaxing process is carried out by at least one of the following methods: storing in a closed container and stirring the whole container, pulverizing using a mortar and pestle, and stirring and pulverizing using a crusher. The method described in [8].

従来のカラフル黒目漆の方法は、生漆を精製して得られる透黒目漆に色素を混合するため、生産効率が低く産業化が困難であった。一方、本発明の方法によれば、生漆にあらかじめ着色剤を混合して減圧蒸留により精製処理を行うことができるため、カラフル黒目漆を短時間で簡便に製造できる。したがって、本発明は、カラフル黒目漆の量産を実現できる技術として期待される。 The conventional method for producing colorful Kurome lacquer involves mixing pigments into clear Kurome lacquer obtained by refining raw lacquer, which has low production efficiency and makes it difficult to industrialize. On the other hand, according to the method of the present invention, a coloring agent can be mixed in advance with raw lacquer and the purification treatment can be performed by distillation under reduced pressure, so colorful black-eyed lacquer can be easily produced in a short time. Therefore, the present invention is expected to be a technology that can realize the mass production of colorful Kurome lacquer.

〔カラフル黒目漆の製造方法〕
-原料生漆液-
原料生漆液は、生漆を含み、着色剤をさらに含んでもよい。
[Production method of colorful Kurome lacquer]
- Raw lacquer liquid -
The raw raw lacquer liquid contains raw lacquer and may further contain a coloring agent.

生漆は、ウルシの樹液に由来する成分を少なくとも含む物質であり、通常は液体である。生漆は、ウルシの樹木から採取される天然樹液、合成品、及びそれらの混合物のいずれを含むものでもよい。 Raw lacquer is a substance that contains at least components derived from sumac sap, and is usually liquid. Raw lacquer may contain any of natural sap collected from sumac trees, synthetic products, and mixtures thereof.

漆の樹木は、ウルシ科(Anacardiaceae)に属する植物の樹木である。ウルシ科植物の生育地は、一般に日本、韓国、中国、東南アジアであるが、原料生漆の産地は特に限定されない。ウルシ科植物としては、例えば、ウルシオールを主成分として含む植物(Toxicodendron vernicifera、産地:中国、日本、韓国)、ラッコールを主成分として含む植物(T.succedanea、産地:ベトナム、台湾)、チチオールを主成分として含む植物(Gluta usitata、産地:ミャンマー、カンボジア、タイ)の3種類が挙げられる。 The lacquer tree is a plant tree belonging to the Anacardiaceae family. The habitats of plants in the sumac family are generally Japan, Korea, China, and Southeast Asia, but the origin of the raw raw lacquer is not particularly limited. Examples of plants in the Anamondaceae family include plants containing urushiol as a main component (Toxicodendron vernicifera, production areas: China, Japan, Korea), plants containing lacquer as a main component (T. succedanea, production areas: Vietnam, Taiwan), and thithiol. There are three types of plants (Gluta usitata, produced in Myanmar, Cambodia, and Thailand) that contain it as a main ingredient.

着色剤は、漆の着色成分以外の着色剤であればよく、無機系(例えば鉱物由来)、有機系(例えば、合成色素、植物抽出色素)のいずれでもよい。無機系着色剤としては、例えば、酸化鉄(例えば、Fe(OH)、Fe)、硫化水銀(HgS)等の無機顔料が挙げられる。有機顔料としては、例えば、クロシン、クロセチン等の色素を含む顔料(例えば、レーキ顔料)が挙げられる。 The coloring agent may be any coloring agent other than the coloring components of lacquer, and may be either inorganic (for example, derived from minerals) or organic (for example, synthetic pigments or plant-extracted pigments). Examples of the inorganic colorant include inorganic pigments such as iron oxide (eg, Fe(OH) 2 , Fe 2 O 3 ) and mercury sulfide (HgS). Examples of organic pigments include pigments containing dyes such as crocin and crocetin (for example, lake pigments).

酸化鉄としてのFe(OH)は、高度に精製されていること(不純物を実質的に含まないこと)が好ましい。不純物としては、例えば、水不溶性成分(例、水不溶性の酸化鉄化合物)が挙げられる。このようなFe(OH)は、例えば、以下の方法により得ることができる。硫酸鉄(FeSO)に水酸化ナトリウム(NaOH)を作用させて調製することが好ましい。例えば、硫酸鉄水溶液に水酸化ナトリウム水溶液を混合し、硫酸鉄である黒緑色の沈殿を発生させ、必要に応じて水で洗浄し、同時に生じる硫酸ナトリウム(NaSO)を除去する方法が挙げられる。硫酸ナトリウムの除去は、塩化バリウム(BaCl)を添加して、硫酸バリウム(BaSO)としての沈殿が生じないことにより確認できる。反応後(洗浄及び/又は硫酸ナトリウム除去確認後)の酸化鉄は、さらに、脱水処理(例えば、ろ紙を接触させる、又は、遠心分離する)により、Fe(OH)沈殿を回収する。これにより、水分量を低減できるので、凝集反応の抑制、減圧蒸留の効率化(時間短縮など)が可能である。 Fe(OH) 2 as iron oxide is preferably highly purified (substantially free of impurities). Examples of impurities include water-insoluble components (eg, water-insoluble iron oxide compounds). Such Fe(OH) 2 can be obtained, for example, by the following method. Preferably, it is prepared by reacting iron sulfate (FeSO 4 ) with sodium hydroxide (NaOH). For example, there is a method in which a sodium hydroxide aqueous solution is mixed with an aqueous iron sulfate solution to generate a black-green precipitate of iron sulfate, which is washed with water if necessary to remove the sodium sulfate (Na 2 SO 4 ) that is produced at the same time. Can be mentioned. Removal of sodium sulfate can be confirmed by addition of barium chloride (BaCl 2 ) and no precipitation as barium sulfate (BaSO 4 ). The iron oxide after the reaction (after washing and/or confirmation of removal of sodium sulfate) is further subjected to dehydration treatment (for example, by contacting with filter paper or centrifuging) to recover Fe(OH) 2 precipitate. This makes it possible to reduce the amount of water, thereby making it possible to suppress aggregation reactions and improve the efficiency of vacuum distillation (shortening the time, etc.).

本明細書において、無添加の原料生漆より調製される黒目漆を、透黒目漆と称し、着色剤を含むカラフル黒目漆と区別することがある。着色剤は、原料生漆液に含まれてもよいし、原料生漆液の減圧蒸留工程、及び必要に応じて行うなやし工程の後に得られる透黒目漆に添加されてもよい。カラフル黒目漆は、その着色剤の種類により、様々な色相を有する。その色相、着色剤の種類により、例えば、弁柄黒目漆、呂色黒目漆、朱色黒目漆、蝋色黒目漆、梨子地黒目漆、牡丹黒目漆と称されることがある。 In this specification, Kurome lacquer prepared from additive-free raw raw lacquer is sometimes referred to as transparent Kurome lacquer, and may be distinguished from colorful Kurome lacquer containing colorants. The coloring agent may be included in the raw raw lacquer solution, or may be added to the transparent black-eye lacquer obtained after the vacuum distillation process of the raw raw lacquer liquor and the optional soothing process. Colorful Kurome lacquer has various hues depending on the type of colorant used. Depending on its hue and the type of coloring agent, it is sometimes called, for example, Bengara Kurome lacquer, Roiro Kurome lacquer, vermilion Kurome lacquer, Roki Kurome lacquer, Nashiji Kurome lacquer, or Botan Kurome lacquer.

原料生漆液における着色剤の含有量は、着色剤の種類によって異なり一般化は難しいが、一例を挙げると、添加対象である漆(生漆又は透黒目漆)100重量%に対し、通常、5重量%以上、好ましくは6重量%以上、より好ましくは7重量%以上である。上限は、通常、150重量%以下、140重量%以下、130重量%以下、100重量%以下、70重量%以下、65重量%以下、又は60重量%以下である。生漆の場合、生漆100重量%に対し、通常、5重量%以上、好ましくは6重量%以上、より好ましくは7重量%以上である。上限は、70重量%以下、好ましくは65重量%以下、より好ましくは60重量%以下である。 The content of coloring agent in the raw raw lacquer solution varies depending on the type of colorant, and it is difficult to generalize, but to give an example, it is usually 5% by weight for 100% by weight of the lacquer to be added (raw lacquer or transparent black lacquer). % or more, preferably 6% by weight or more, more preferably 7% by weight or more. The upper limit is usually 150% by weight or less, 140% by weight or less, 130% by weight or less, 100% by weight or less, 70% by weight or less, 65% by weight or less, or 60% by weight or less. In the case of raw lacquer, the content is usually 5% by weight or more, preferably 6% by weight or more, and more preferably 7% by weight or more, based on 100% by weight of raw lacquer. The upper limit is 70% by weight or less, preferably 65% by weight or less, more preferably 60% by weight or less.

-減圧蒸留-
減圧蒸留処理を行うことにより、従来の方法よりも短時間で、かつかぶれの発症を抑制しながら安全に良好な品質のカラフル黒目漆を得ることができる。
-Vacuum distillation-
By performing vacuum distillation treatment, it is possible to safely obtain high-quality colorful black-eye lacquer in a shorter time than with conventional methods, while suppressing the onset of rashes.

減圧蒸留の条件は、特に限定されないが、一例を挙げると以下のとおりである。圧力は、蒸気圧より25hPa以上減圧することが好ましく、30hPa以上がより好ましい。減圧条件は、蒸気圧より25~60hPa低下させることが好ましく、30~50hPa低下させることがより好ましい。これにより、原料生漆に含まれる低沸点の揮発性テルペン類、ガス成分、水分を短時間で十分に除去できる。 The conditions for vacuum distillation are not particularly limited, but an example is as follows. The pressure is preferably reduced by 25 hPa or more, more preferably 30 hPa or more, from the vapor pressure. The reduced pressure condition is preferably 25 to 60 hPa lower than the vapor pressure, more preferably 30 to 50 hPa lower than the vapor pressure. This makes it possible to sufficiently remove low-boiling point volatile terpenes, gas components, and moisture contained in the raw raw lacquer in a short time.

減圧蒸留の温度は、通常、室温以下(例えば、38℃以下、35℃以下又は30℃以下)であり、好ましくは20~35℃、より好ましくは20~30℃である。これにより、原料生漆に含まれるラッカーゼの変性による失活を抑制できる。 The temperature of vacuum distillation is usually below room temperature (eg, below 38°C, below 35°C, or below 30°C), preferably between 20 and 35°C, more preferably between 20 and 30°C. Thereby, deactivation due to denaturation of laccase contained in the raw raw lacquer can be suppressed.

減圧蒸留の時間は、30分以上が好ましく、40分以上がより好ましい。上限は特に制限はないが、通常は200分以下、180分以下、120分以下、好ましくは80分以下である。これにより、適切な水分量のカラフル黒目漆を得ることができる。 The time for vacuum distillation is preferably 30 minutes or more, more preferably 40 minutes or more. The upper limit is not particularly limited, but is usually 200 minutes or less, 180 minutes or less, 120 minutes or less, preferably 80 minutes or less. This makes it possible to obtain colorful black-eyed lacquer with an appropriate moisture content.

減圧蒸留中の水分量を計測管理し、所望の水分量(例えば、3.5重量%以下、3.2重量%以下又は3重量%以下、好ましくは2.5重量%以下、又は2重量%以下)となった時点で減圧蒸留を終了し産物を回収してもよい。水分量の計測法としては、例えば、乾燥減量法、近赤外分光法、ガスクロマトグラフ法及びカールフィッシャー法が挙げられ、これらのうちサンプルが少量でも正確な定量が可能であり、感度がよいこと、再現性に優れることから、カールフィッシャー法が好ましい。カールフィッシャー法は、滴定セル内でカールフィッシャー試薬(ヨウ化物イオン、二酸化硫黄、アルコールを主成分とする電解液)が、メタノールの存在下で水と特異的に反応することを利用して、物質中の水分を定量する方法である。カールフィッシャー法は、滴定の進め方により容量滴定法及び電量滴定法に分類され、容量滴定法が好ましい。容量滴定法は、滴定フラスコに試料に適した脱水溶剤(例えば、無水分子ふるい)を入れておき、滴定剤で無水状態にしてから試料を加え、あらかじめ力価(mgHO/mL)を標定しておいた滴定剤を用いて滴定を行い、その滴定量(mL)から試料中の水分量を重量%として正確に求める。 The moisture content during vacuum distillation is measured and managed, and the desired moisture content (for example, 3.5% by weight or less, 3.2% by weight or less, or 3% by weight or less, preferably 2.5% by weight or less, or 2% by weight) (below), the vacuum distillation may be terminated and the product may be recovered. Methods for measuring moisture content include, for example, the loss on drying method, near-infrared spectroscopy, gas chromatography, and Karl Fischer method, and among these methods, accurate quantification is possible even with a small sample, and the sensitivity is good. The Karl Fischer method is preferred because of its excellent reproducibility. The Karl Fischer method utilizes the fact that the Karl Fischer reagent (an electrolyte containing iodide ions, sulfur dioxide, and alcohol as its main components) specifically reacts with water in the presence of methanol in a titration cell. This is a method to quantify the moisture content. The Karl Fischer method is classified into a volumetric titration method and a coulometric titration method depending on the titration procedure, with the volumetric titration method being preferred. In the volumetric titration method, a titration flask is filled with a dehydrated solvent suitable for the sample (e.g., anhydrous molecular sieves), the titration agent is used to make it anhydrous, the sample is added, and the titer (mgH 2 O/mL) is standardized in advance. Titration is performed using the titrant that has been prepared in advance, and the water content in the sample is accurately determined as weight % from the titration (mL).

-なやし処理(生漆の前処理の例)-
原料生漆液、又は、着色剤添加前の生漆は、前処理(なやし処理)を経ていてもよい。なやし処理を行うことにより、生漆の中に存在する水分と水溶性タンパク質を含む大きさの異なる種類のミセル粒子(水相)を破壊し、ウルシオールを含む油相にミセルを均一に分散させることができ、これにより減圧蒸留の際の水分回収を促進できる。また、得られるカラフル黒目漆の光沢及び/又は粘度を高めることができる。
- Nayashi treatment (example of pre-treatment of raw lacquer) -
The raw lacquer solution or the raw lacquer before addition of the colorant may be subjected to pretreatment (calming treatment). By performing the soothing treatment, the micelle particles of different sizes (aqueous phase) containing water and water-soluble proteins that exist in raw lacquer are destroyed, and the micelles are uniformly dispersed in the oil phase containing urushiol. This can promote water recovery during vacuum distillation. Moreover, the gloss and/or viscosity of the obtained colorful black-eye lacquer can be increased.

なやし処理の方法としては、例えば、原料生漆を撹拌、粉砕する方法が挙げられ、密閉容器へ格納し容器ごと撹拌(例えば、回転撹拌)する方法、又は、乳鉢と乳棒を用いて粉砕する方法、又は擂潰機を用いて粉砕する方法が好ましい。密閉容器を用いる方法の場合、減圧蒸留の際に用いる装置が備える容器をそのまま用いてもよい。なやし処理の温度条件は、減圧蒸留よりも低温であることが好ましく、通常、35℃以下が好ましく、34℃以下、又は33℃以下がより好ましく、32℃以下、31℃以下又は30℃以下が更に好ましい。下限は、通常、20℃以上、好ましくは22℃以上、又は23℃以上、より好ましくは24℃以上、又は25℃以上である。圧力は、通常、常圧(大気圧、通常は1atm)で行い、減圧及び加圧処理は行わないことが好ましい。処理時間は、通常、15分以上、好ましくは20分以上である。上限は、250分以下、200分以下、180分以下、100分以下、好ましくは90分以下、より好ましくは80分以下である。 Examples of methods for soothing treatment include stirring and pulverizing the raw raw lacquer; storing it in an airtight container and stirring the whole container (e.g., rotary stirring); or pulverizing it using a mortar and pestle. or a method of crushing using a grinder is preferred. In the case of a method using a closed container, the container provided in the apparatus used for vacuum distillation may be used as is. Temperature conditions for the tempering treatment are preferably lower than that of vacuum distillation, usually preferably 35°C or lower, more preferably 34°C or lower, or 33°C or lower, 32°C or lower, 31°C or lower, or 30°C. The following are more preferable. The lower limit is usually 20°C or higher, preferably 22°C or higher, or 23°C or higher, more preferably 24°C or higher, or 25°C or higher. The pressure is usually normal pressure (atmospheric pressure, usually 1 atm), and it is preferable that pressure reduction and pressure treatment are not performed. The treatment time is usually 15 minutes or more, preferably 20 minutes or more. The upper limit is 250 minutes or less, 200 minutes or less, 180 minutes or less, 100 minutes or less, preferably 90 minutes or less, more preferably 80 minutes or less.

乳鉢と乳棒を用いる処理、又は擂潰機を用いる処理の、処理時間は、それぞれ通常、10分以上、好ましくは15分以上である。上限は特にないが、通常、60分以下、50分以下、好ましくは40分以下である。 The processing time for the processing using a mortar and pestle or the processing using a crusher is usually 10 minutes or more, preferably 15 minutes or more. There is no particular upper limit, but it is usually 60 minutes or less, 50 minutes or less, preferably 40 minutes or less.

擂潰機としては、鉢と、鉢内部で自公転し鉢内容物を圧接可能な複数の棒(杵)を有する撹拌擂潰機(例えば、特開昭51-110756号公報、石川式撹拌擂潰機(石川工場社製))が好ましい。これにより、撹拌及び/又は粉砕(例えば、摩砕)を効率よく実施できる。撹拌擂潰機を用いる場合、回転数は、20rpm以上が好ましく、25rpm以上がより好ましい。上限は、30rpm以下が好ましい。 As a crusher, an agitator crusher having a bowl and a plurality of rods (pestles) that rotate around and around the inside of the bowl and can press the contents of the bowl (for example, Japanese Patent Application Laid-Open No. 110756/1983, Ishikawa type stirring crusher) A crusher (manufactured by Ishikawa Factory Co., Ltd.) is preferred. Thereby, stirring and/or grinding (for example, grinding) can be carried out efficiently. When using a stirrer and crusher, the rotation speed is preferably 20 rpm or more, more preferably 25 rpm or more. The upper limit is preferably 30 rpm or less.

なやし処理は、乳鉢と乳棒を用いる処理及び擂潰機を用いる処理のいずれか;若しくは、密閉容器を用いる処理と、乳鉢と乳棒を用いる処理、又は擂潰機を用いる処理と、の組み合わせが好ましい。 Nail treatment is either a process using a mortar and pestle or a process using a crusher; or a combination of a process using a closed container and a process using a mortar and pestle or a process using a crusher. is preferred.

なやし工程の温度条件は、35℃以下が好ましい。これにより、低温で短時間(通常、2時間以内)に水分を約3%以下まで除去でき、そのためラッカーゼ変性を回避できる。 The temperature condition for the soothing step is preferably 35° C. or lower. This allows water to be removed to about 3% or less in a short period of time (usually within 2 hours) at low temperatures, thereby avoiding laccase denaturation.

-ろ過(生漆の前処理の例)-
原料生漆液、又は、着色剤添加前の生漆は、ろ過処理を経ていてもよい。ろ過処理により、生漆に含まれる不溶性成分を除去できる。
-Filtration (example of pre-treatment of raw lacquer)-
The raw lacquer solution or the raw lacquer before adding a colorant may be subjected to a filtration treatment. Filtration treatment can remove insoluble components contained in raw lacquer.

ろ過処理は、少なくとも1回行えばよく、2回以上行ってもよい。ろ過の時期は、減圧処理の前、又は後に行うことができ、なやし処理を行う場合にはその前に行うことが好ましい。ろ過処理により、原料生漆に含まれ得る不純物を、さらになやし処理を行う場合にはその際に生じ得る不溶性メラニン色素等を含む不溶性成分も、除去できる。これらの光散乱を生じるおそれのある成分を除去できるので、得られるカラフル黒目漆の光沢及び/又は艶感をより高めることができる。また、なやし処理の時間、種類などの条件を調整することにより、得られるカラフル黒目漆の光沢及び/又は艶感を所望に応じて調整できる。なお、本明細書において、減圧蒸留前に先立ちろ過を行った生漆を、漉味生漆と呼び、ろ過未処理の生漆である荒味生漆と区別することがある。 The filtration treatment may be performed at least once, or may be performed two or more times. The filtration can be performed before or after the depressurization treatment, and in the case of performing the decompression treatment, it is preferably performed before the decompression treatment. By the filtration treatment, impurities that may be contained in the raw raw lacquer can be removed, and in the case where a soothing treatment is performed, insoluble components such as insoluble melanin pigments that may be generated at that time can also be removed. Since these components that may cause light scattering can be removed, the gloss and/or luster of the resulting colorful Kurome lacquer can be further enhanced. Furthermore, by adjusting the conditions such as the time and type of soothing treatment, the gloss and/or luster of the resulting colorful Kurome lacquer can be adjusted as desired. In this specification, raw lacquer that has been filtered prior to vacuum distillation is referred to as lacquer-flavored raw lacquer, and may be distinguished from coarse-flavored raw lacquer, which is unfiltered raw lacquer.

ろ過に用いるろ材は特に限定されず、例えば、綿、ガーゼ等の布、ろ紙(例えば、和紙、再生セルロース紙、試験用ろ紙)等の紙、金網等の金属が挙げられる。ろ材は、2以上のろ材の組み合わせでもよい。中でも、綿、ろ紙、又はこれらの組み合わせが好ましい。綿、ろ紙は、従来より漉味生漆の製造において用いられてきたろ材であり、好ましく用いられる。ろ過の方法は、ろ材に適した条件で行えばよい。綿を用いる場合、例えば、綿を適量(例えば、漆の重量の5~20重量%に相当する量)漆に浸漬して静置(例えば、10~20分)する方法が挙げられる。ろ紙を用いる場合、例えば、ろ紙の上面に漆を注ぎ、下面に染み出たろ液を絞って回収する方法が挙げられる。綿とろ紙の組み合わせを用いる場合、綿によるろ過とろ紙によるろ過の順序は特に限定されないが、前者を先に行うことが好ましい。これにより、綿を浸漬した状態のサンプルをろ紙の上に注ぎ、ろ紙を通過した液(必要に応じてろ紙を絞ってもよい)として処理後の漆を回収できる。 The filter medium used for filtration is not particularly limited, and examples thereof include cloth such as cotton and gauze, paper such as filter paper (for example, Japanese paper, regenerated cellulose paper, and test filter paper), and metal such as wire mesh. The filter medium may be a combination of two or more filter mediums. Among these, cotton, filter paper, or a combination thereof is preferred. Cotton and filter paper are filter media that have traditionally been used in the production of lacquer-flavored raw lacquer, and are preferably used. The filtration method may be carried out under conditions suitable for the filter medium. When cotton is used, for example, a method of soaking an appropriate amount of cotton (for example, an amount corresponding to 5 to 20% by weight of the weight of the lacquer) in lacquer and leaving it to stand (for example, 10 to 20 minutes) can be mentioned. When using filter paper, for example, lacquer is poured onto the top surface of the filter paper, and the filtrate that seeps out from the bottom surface is squeezed and collected. When using a combination of cotton and filter paper, the order of filtration through cotton and filtration through filter paper is not particularly limited, but it is preferable to perform the former first. Thereby, the sample in which the cotton is soaked can be poured onto the filter paper, and the treated lacquer can be recovered as a liquid that has passed through the filter paper (the filter paper may be squeezed if necessary).

生漆は、ろ過処理及びなやし処理およびのいずれかを経ていることが好ましく、両方を経ていることがより好ましい。 It is preferable that the raw lacquer has undergone either a filtration treatment or a soothing treatment, and more preferably both.

本発明の方法により、カラフル黒目漆を、短時間で、安定的に得ることができる。カラフル黒目漆は、用いる着色料に応じた発色を示し、良好な光沢、艶感及び/又は粘度を示すことができる。 By the method of the present invention, colorful Kurome lacquer can be stably obtained in a short time. Colorful Kurome lacquer exhibits color development depending on the colorant used, and can exhibit good gloss, luster, and/or viscosity.

実施例1(サンプル1:弁柄黒目漆)
〔なやし処理〕
表1に示す量の城口漉味生漆(辻田漆店製、2022年1月27日精製、以下同じ)及び弁柄顔料(Bura社)を、ガラス製乳鉢(200ml,Sigma-Aldrich社)に加えた後、ガラス製乳棒で室温下20~30分間強く粉砕してウルシ属のミセルとベンガラ粉末が完全に分散して気泡が発生しないとき、Diaphragm式真空ポンプ(NVP-2100,東京理化器械社製)及びウォーターバスを備えたロータリーエバポーター(東京理化器械社製)の減圧フラスコ中に投入し、系内をアルゴン置換して、35℃で20~40分間、常圧で撹拌を行い、なやし処理済みのサンプルを得た。
Example 1 (Sample 1: Bengara Kurome lacquer)
[Soothing treatment]
The amounts of Shiroguchi lacquer raw lacquer (manufactured by Tsujita Urushiten, refined on January 27, 2022, the same applies hereinafter) and Bengara pigment (Bura) shown in Table 1 were placed in a glass mortar (200ml, Sigma-Aldrich). After adding the mixture, grind it strongly with a glass pestle for 20 to 30 minutes at room temperature. ) and a rotary evaporator (manufactured by Tokyo Rikakikai Co., Ltd.) equipped with a water bath, the system was replaced with argon, and stirred at 35°C for 20 to 40 minutes at normal pressure. A palm-treated sample was obtained.

〔減圧蒸留〕
なやし処理済みのサンプルを、フラスコ内にそのまま維持し、系内をアルゴン置換して蒸気圧から約40hPa減圧し、気泡が発生しなくなるまで35℃で減圧蒸留を行い(蒸留時間:70分間)、サンプル1(弁柄黒目漆)を回収した(表1)。
[Vacuum distillation]
The parched sample was maintained in the flask, the system was replaced with argon, the vapor pressure was reduced by approximately 40 hPa, and vacuum distillation was performed at 35°C until no bubbles were generated (distillation time: 70 minutes). ), Sample 1 (Begara Kurome lacquer) was collected (Table 1).

カールフィッシャー水分測定器(メトローム社製)を用いて減圧蒸留開始前及び終了後のサンプルのそれぞれの水分量を測定した(n=3)。
測定条件は、以下のとおりであった。
減圧蒸留開始時のサンプル重量:50mg±5mg
温度:180℃
抽出時間:400秒
流速:80ml/分
反応終了時、気流を停止し、水分量を測定後、水分測定器からサンプルを取り出した。
流速:80ml/分
Using a Karl Fischer moisture meter (manufactured by Metrohm), the moisture content of each sample was measured before and after the vacuum distillation was started (n=3).
The measurement conditions were as follows.
Sample weight at the start of vacuum distillation: 50mg±5mg
Temperature: 180℃
Extraction time: 400 seconds Flow rate: 80 ml/min At the end of the reaction, the air flow was stopped, and after measuring the moisture content, the sample was taken out from the moisture meter.
Flow rate: 80ml/min

実施例2(サンプル2:呂色黒目漆)
弁柄顔料の代わりに、表1に示す量のFeSO及びNaOHを用いたほかは、実施例1と同様に行い、ダークブラックの呂色黒目漆(サンプル2)を得た。
Example 2 (Sample 2: Roiro Kurome lacquer)
The same procedure as in Example 1 was carried out except that FeSO 4 and NaOH in the amounts shown in Table 1 were used instead of the Bengara pigment, to obtain dark black Roiro Kurome lacquer (Sample 2).

実施例3(サンプル3:朱色黒目漆)
弁柄顔料の代わりに、表1に示す量の日華朱(HgS、Yamamoto Scinnabar社)を用いたほかは、実施例1と同様に行い、朱色黒目漆(サンプル3)を得た。
Example 3 (Sample 3: Vermilion black lacquer)
In place of the Bengara pigment, the procedure was repeated in the same manner as in Example 1, except that Nikka shu (HgS, Yamamoto Scinnabar) was used in the amount shown in Table 1, to obtain vermilion Kurome lacquer (sample 3).

実施例4(サンプル4:桃色黒目漆)
弁柄顔料の代わりに、表1に示す量の牡丹顔料(レーキ顔料、パーマネントカラー黒函牡丹、堤淺吉漆店)を用いたほかは、実施例1と同様に行った。
Example 4 (Sample 4: Pink black lacquer)
The same procedure as in Example 1 was carried out, except that instead of Bengara pigment, Botan pigment (Lake pigment, Permanent Color Kurobako Botan, Tsutsumi Asakichi Lacquer Store) was used in the amount shown in Table 1.

参考例1~2(サンプル5~6:透黒目漆)
顔料を添加しなかったほかは、実施例1と同様に行った。
Reference examples 1 to 2 (Samples 5 to 6: Clear black lacquer)
The same procedure as in Example 1 was carried out except that no pigment was added.

比較例1(サンプル7:市販透黒目漆)
顔料を添加しなかったほかは、実施例1と同様に行った。
透黒目漆(辻田商店)をサンプル7とした。
Comparative Example 1 (Sample 7: Commercially available transparent black-eye lacquer)
The same procedure as in Example 1 was carried out except that no pigment was added.
Sample 7 was transparent Kurome lacquer (Tsujita Shoten).

(光沢度)
サンプル1~7の光沢度を以下の手順で測定した。木製の平板に城口荒味生漆で下塗して25℃、湿度75%で12時間乾燥させた。続いて、城口荒味生漆と砥粉(錆)(生漆:砥粉=8:2の混合液)で中塗して、25℃、湿度75%で12時間乾燥させた。続いて、城口呂色黒目漆(辻田漆店、2021年9月精製)で上塗して、25℃、湿度75%で12時間乾燥させた。その後、表面をサンドペーパーで研磨した。塗布及び研磨終了後に、木製の平板をテープで区画し(1区画あたり約5cm×約10cm)、各区画内にサンプル1~7をそれぞれ1滴滴下し、均一になるようコーティングし、25℃、湿度75%で12時間乾燥させた。その後、ハンディ光沢計グロスチェッカIG-331(HORIBA社製)を用いて光沢度(測定角60°、バルブ90)を3回測定し、その平均値を光沢度とした(表1)。なお、コントロールの条件として、測定角60°で90となるように設定した。
(Glossiness)
The glossiness of Samples 1 to 7 was measured using the following procedure. A wooden board was prime coated with Shiroguchi Arami Nama Urushi and dried at 25°C and 75% humidity for 12 hours. Subsequently, an intermediate coating was applied with Shiroguchi rough raw lacquer and abrasive powder (rust) (raw lacquer: abrasive powder = 8:2 mixture) and dried at 25° C. and 75% humidity for 12 hours. Next, it was overcoated with Shiroguchiro Irokurome lacquer (Tsujita Urushiten, refined in September 2021) and dried at 25°C and 75% humidity for 12 hours. After that, the surface was polished with sandpaper. After coating and polishing, divide the wooden plate into sections with tape (approximately 5 cm x approximately 10 cm per section), drop one drop of Samples 1 to 7 into each section, coat uniformly, and heat at 25°C. It was dried for 12 hours at a humidity of 75%. Thereafter, the glossiness (measurement angle 60°, bulb 90) was measured three times using a handy glossmeter Gloss Checker IG-331 (manufactured by HORIBA), and the average value was taken as the glossiness (Table 1). Note that the control conditions were set to 90 at a measurement angle of 60°.

(粘度)
ガラス板に各サンプルを1滴垂らし、室温で30分放置した。スポットからストリームの終点までの距離を測定し、粘度を判断した(表1に、粘度の高い順に数字を示した)。
(viscosity)
One drop of each sample was placed on a glass plate and left at room temperature for 30 minutes. The distance from the spot to the end of the stream was measured to determine the viscosity (numbers are shown in Table 1 in descending order of viscosity).

Figure 2023164367000001
Figure 2023164367000001

カラフル黒目漆であるサンプル1~4は、透黒目漆であるサンプル5、6と比較して光沢度が高い傾向にあった。サンプル1~4の粘度は、市販品であるサンプル7と比較して高く、いずれも許容範囲内であった(表1)。 Samples 1 to 4, which were colorful black-eyed lacquer, tended to have higher gloss than samples 5 and 6, which were transparent black-eyed lacquer. The viscosities of Samples 1 to 4 were higher than that of Sample 7, a commercially available product, and all were within the acceptable range (Table 1).

なお、実施例1において、減圧蒸留における減圧後の圧力を約25hPaに変更し、蒸留時間を約70~90分間に調整した場合も、実施例1と同様の結果が得られた。 In Example 1, the same results as in Example 1 were also obtained when the pressure after reduced pressure in vacuum distillation was changed to about 25 hPa and the distillation time was adjusted to about 70 to 90 minutes.

実施例5(精製Fe(OH)2を用いた呂色黒目漆の調製)
〔FeSOの精製〕
FeSO 162mmol(45g)(Sigma-Aldrich,Catalogue No.7782-63-0)に蒸留水500mlを添加し、撹拌した。得られたFeSO懸濁液を、ろ紙(ADVANTEC(登録商標)filter paper 2)を用いてろ過して酸化鉄(溶解しない)を除去し、液相を分離した。この液相を、Diaphragm式真空ポンプ(NVP-2100,東京理化器械社製)及びウォーターバスを備えたロータリーエバポーター(東京理化器械社製)の減圧フラスコ中に投入し、系内をアルゴン置換して、35℃で2時間撹拌を行った。回収された緑色の結晶42gは、精製FeSOであった。
Example 5 (Preparation of Roirokurome lacquer using purified Fe(OH) 2 )
[Purification of FeSO4 ]
500 ml of distilled water was added to 162 mmol (45 g) of FeSO 4 (Sigma-Aldrich, Catalog No. 7782-63-0) and stirred. The resulting FeSO 4 suspension was filtered using filter paper (ADVANTEC® filter paper 2) to remove iron oxide (not dissolved) and the liquid phase was separated. This liquid phase was put into a vacuum flask of a rotary evaporator (manufactured by Tokyo Rikakikai Co., Ltd.) equipped with a Diaphragm vacuum pump (NVP-2100, Tokyo Rikakikai Co., Ltd.) and a water bath, and the system was replaced with argon. The mixture was stirred at 35°C for 2 hours. The 42 g of green crystals recovered were purified FeSO4 .

〔Fe(OH)2の調製〕
上述の手順で得られた精製FeSO 4.2mmol(1.16g)を蒸留水100mlに溶解させ、FeSO溶液を調製した。一方、NaOH 8.4mmol(0.336g)を、蒸留水100mlに溶解させてNaOH溶液を調製し、これをFeSO溶液に加えながらよく撹拌し均一な沈殿(黒緑色)を生成させた後、1時間放置した。放置終了後、上清のpHが中性~弱酸性(約5~6.5)となるように、FeSO溶液を添加した。さらに1時間放置後、上清を除去し、副生成物であるNa2SOの除去のため、残渣を蒸留水で5回以上洗浄し、洗浄後の残渣を以下の工程でFe(OH)2として用いた。洗浄によりサンプルからNa2SOが除去されていることは、0.1MBaCl2水溶液を洗浄液と1:1で混合した際に白色沈殿(BaSO)の発生がないことにより確認した。洗浄後の残渣は、室温で200rpmの条件で遠心処理し、脱水した。
[Preparation of Fe(OH) 2 ]
4.2 mmol (1.16 g) of purified FeSO 4 obtained by the above procedure was dissolved in 100 ml of distilled water to prepare a FeSO 4 solution. On the other hand, 8.4 mmol (0.336 g) of NaOH was dissolved in 100 ml of distilled water to prepare a NaOH solution, and this was added to the FeSO 4 solution while stirring well to generate a uniform precipitate (black green color). It was left for 1 hour. After standing, a FeSO 4 solution was added so that the pH of the supernatant was neutral to weakly acidic (approximately 5 to 6.5). After standing for another hour, the supernatant was removed, and the residue was washed with distilled water at least 5 times to remove the byproduct Na 2 SO 4 . The residue after washing was converted to Fe(OH) in the following step. It was used as 2 . The removal of Na 2 SO 4 from the sample by washing was confirmed by the fact that no white precipitate (BaSO 4 ) was generated when 0.1 M BaCl 2 aqueous solution was mixed with the washing solution at a ratio of 1:1. The residue after washing was dehydrated by centrifugation at room temperature and 200 rpm.

〔呂色黒目漆の調製〕
上述の手順で得られたFe(OH)2 1gを、実施例1と同じ漉味生漆50gに添加した(漉味生漆に対しFe(OH)2 2重量%)。粉砕時間を15分としたことのほかは、実施例1と同様の粉砕処理を行い、続いて、処理時間2.5時間としたことのほかは、実施例1と同様の減圧蒸留及び水分の確認を行い、呂色黒目漆を得た。減圧蒸留前の水分量27.74%、減圧蒸留後の水分量2.15%、光沢度115であったことから、実施例1と比較して光沢が顕著に向上していたことが分かった。
[Preparation of Roirokurome lacquer]
1 g of Fe(OH) 2 obtained by the above procedure was added to 50 g of the same lacquer-flavored raw lacquer as in Example 1 (2% by weight of Fe(OH) 2 based on the lacquer-flavored raw lacquer). The same pulverization treatment as in Example 1 was carried out, except that the pulverization time was 15 minutes, and then the same vacuum distillation and water removal as in Example 1 were carried out, except that the treatment time was 2.5 hours. After confirmation, we obtained Roirokurome lacquer. The moisture content before vacuum distillation was 27.74%, the moisture content after vacuum distillation was 2.15%, and the gloss was 115, indicating that the gloss was significantly improved compared to Example 1. .

実施例6~9(白色漆の調製)
表2に示す量の城口漉味生漆(辻田漆店製、2022年1月27日精製、以下同じ)を、石川式撹拌擂潰機(石川工場社製、竪型(プーリー式)22号;機械の外形寸法:長さ610mm、幅610mm、高さ1450mm;磁器鉢(内径305mm、深さ170mm、使用容積4.0L)、T型磁器杵(2本)、かき板(木製)を装備;電動機(モーター単相100V 0.2kW);杵が公転1周に対し自転約2.4周の速さで同じ方向に回転)(鉢は、前方への引き出し、及び引き出した状態で前傾し鉢内容物を容易に取り出せるよう改造)の鉢に注入し、室温で、杵の回転数26rpmで15分処理した。減圧蒸留を開始する前にエバポレータの減圧が正常に動作していることを確認するために、空のフラスコをエバポレータに取り付けた後、15分間25hPaの減圧処理を行った。正常に減圧処理が達成されたことを確認した後、擂潰処理済みのサンプルを、擂潰機の鉢を前方へ引き出し前傾させて取り出し、フラスコに入れ、エバポレータに付着し、ウォーターバスの温度を約15℃に調整し、15分間で25hpaまで減圧し、テルペンなどの低沸点物質を除去した。15分後(25hpaに到達した後)は、ウォーターバス温度を35℃まで徐々に加熱しながら減圧蒸留し、水分を除去した。2時間で蒸留はほぼ完了したと推測されたが、さらにウォーターバスの温度を38℃に調整して30分減圧蒸留した(エバポレータ処理時間の合計;2.5~3時間)。処理後のサンプルの水分が、カールフィッシャー水分定量器を用いる定量(バイアルにサンプルを注入し、180℃、400秒、風速100mL/分の条件で定量)により3%以下であることを確認後、減圧蒸留を止めて精製された黒目漆を回収した。その後、ろ紙(レーヨン製、商品名:美吉野紙(530mm×300mm)、大塚刷毛製造社製)で濾過し、透黒目漆を得た。
Examples 6-9 (Preparation of white lacquer)
The amount of Shiroguchi lacquer raw lacquer shown in Table 2 (manufactured by Tsujita Urushiten, refined on January 27, 2022, the same applies hereinafter) was added to an Ishikawa-type stirring and crushing machine (manufactured by Ishikawa Factory Co., Ltd., vertical type (pulley type) No. 22). External dimensions of the machine: length 610mm, width 610mm, height 1450mm; Equipped with a porcelain pot (inner diameter 305mm, depth 170mm, usable volume 4.0L), T-shaped porcelain pestle (2 pieces), and scraping board (wooden) ; Electric motor (motor single phase 100V 0.2kW); Pestle rotates in the same direction at a rate of about 2.4 revolutions per revolution) (The bowl can be pulled forward and tilted forward when pulled out. The mixture was poured into a pot (modified so that the contents of the pot could be easily taken out) and treated at room temperature with a pestle at 26 rpm for 15 minutes. In order to confirm that the vacuum in the evaporator was operating normally before starting vacuum distillation, an empty flask was attached to the evaporator and then vacuum treatment was performed at 25 hPa for 15 minutes. After confirming that the depressurization process has been successfully achieved, take out the crushed sample by pulling the crusher bowl forward and tilting it forward, placing it in a flask, attaching it to the evaporator, and lowering the temperature of the water bath. The temperature was adjusted to about 15° C., and the pressure was reduced to 25 hpa for 15 minutes to remove low-boiling substances such as terpenes. After 15 minutes (after reaching 25 hpa), water was removed by distillation under reduced pressure while gradually heating the water bath temperature to 35°C. It was estimated that the distillation was almost completed in 2 hours, but the temperature of the water bath was further adjusted to 38° C. and distillation was carried out under reduced pressure for 30 minutes (total evaporator treatment time; 2.5 to 3 hours). After confirming that the moisture content of the sample after processing is 3% or less by quantification using a Karl Fischer moisture meter (injecting the sample into a vial and quantifying it at 180 ° C. for 400 seconds and at a wind speed of 100 mL/min), The vacuum distillation was stopped and the purified Kurome lacquer was collected. Thereafter, it was filtered through a filter paper (made by Rayon, trade name: Miyoshino Paper (530 mm x 300 mm), manufactured by Otsuka Brush Manufacturing Co., Ltd.) to obtain transparent black-eye lacquer.

得られた透黒目漆に対し白色顔料(メーカー名:堤浅吉漆店、商品名:パーマネントカラー)を表2に記載の比率で添加し混合し、白色漆を調製した。 A white pigment (manufacturer name: Tsutsumi Asayoshi Urushiten, product name: Permanent Color) was added and mixed in the ratio shown in Table 2 to the obtained transparent black-eye lacquer to prepare white lacquer.

Figure 2023164367000002
Figure 2023164367000002

得られた白色漆は、艶感が良好であった。 The obtained white lacquer had good gloss.

実施例10(弁柄黒目漆10の製造)
生漆及び弁柄顔料の量を表3に示す量に調整し、実施例6と同様の粉砕処理(ただし、粉砕時間30分)を行った。その後、減圧蒸留時間を3時間としたほかは実施例5と同様の減圧蒸留処理を行った(表3)。
Example 10 (Production of Bengara Kurome Urushi 10)
The amounts of raw lacquer and Bengara pigment were adjusted to the amounts shown in Table 3, and the same pulverization treatment as in Example 6 was performed (however, the pulverization time was 30 minutes). Thereafter, the same vacuum distillation treatment as in Example 5 was performed except that the vacuum distillation time was changed to 3 hours (Table 3).

実施例11(弁柄黒目漆の製造)
生漆の代わりに透黒目漆(いわて漆テック社製)を用いたこと、各原料の使用量を表3のとおりとしたこと、蒸留時間を2.5時間としたことの他は、実施例10と同様に行った(表3)。
Example 11 (Production of Bengara Kurome lacquer)
Example 10 except that transparent black-eye lacquer (manufactured by Iwate Urushi Tech Co., Ltd.) was used instead of raw lacquer, the amounts of each raw material used were as shown in Table 3, and the distillation time was 2.5 hours. It was carried out in the same manner as (Table 3).

Figure 2023164367000003
Figure 2023164367000003

得られた弁柄黒目漆は、良好な光沢度を示した。 The obtained Bengara Kurome lacquer showed good gloss.

実施例12~19(カラフル漆の製造)
実施例6において、顔料及び透黒目漆の量を表4に示す種類及び量としたことの他は、実施例6と同様に行った(表4)。その結果、いずれのカラフル漆も、水分含量が低く、良好な光沢度を示し、回収量が高率であった。
Examples 12 to 19 (manufacture of colorful lacquer)
Example 6 was carried out in the same manner as in Example 6, except that the amounts of pigment and transparent black-eye lacquer were changed to the types and amounts shown in Table 4 (Table 4). As a result, all colorful lacquers had low water content, exhibited good gloss, and had a high recovery rate.

Figure 2023164367000004
Figure 2023164367000004

Claims (9)

生漆を含む原料生漆液を減圧蒸留する工程を含み、着色剤を原料生漆液に添加するか、又は、減圧蒸留後に得られる透黒目漆に添加する、カラフル黒目漆の製造方法。 A method for producing colorful Kurome lacquer, which includes a step of distilling raw raw lacquer containing raw lacquer under reduced pressure, and adding a coloring agent to the raw raw lacquer or to transparent Kurome lacquer obtained after vacuum distillation. 減圧蒸留は、処理後の水分量が3重量%以下となるまで行う、請求項1に記載の製造方法。 The manufacturing method according to claim 1, wherein the vacuum distillation is performed until the water content after treatment becomes 3% by weight or less. 減圧蒸留は、原料生漆液の蒸気圧より25~60hPa減圧して行う、請求項1又は2に記載の製造方法。 The production method according to claim 1 or 2, wherein the vacuum distillation is performed at a pressure of 25 to 60 hPa lower than the vapor pressure of the raw raw lacquer solution. 減圧蒸留は、30分以上行う、請求項1又は2に記載の製造方法。 The manufacturing method according to claim 1 or 2, wherein the vacuum distillation is performed for 30 minutes or more. 減圧蒸留は、20~35℃で行う、請求項1又は2に記載の製造方法。 The production method according to claim 1 or 2, wherein the vacuum distillation is carried out at 20 to 35°C. 着色剤は、無機顔料又は有機顔料である、請求項1又は2に記載の製造方法。 The manufacturing method according to claim 1 or 2, wherein the colorant is an inorganic pigment or an organic pigment. 着色剤は、酸化鉄、硫化水銀、レーキ顔料である、請求項1又は2に記載の製造方法。 The manufacturing method according to claim 1 or 2, wherein the coloring agent is iron oxide, mercury sulfide, or lake pigment. 原料生漆液又は生漆を、35℃以下で常圧下撹拌又は粉砕するなやし処理工程、及び/又は、ろ過処理工程を更に含む、請求項1又は2に記載の製造方法。 The manufacturing method according to claim 1 or 2, further comprising a soothing treatment step of stirring or pulverizing the raw raw lacquer liquid or raw lacquer under normal pressure at 35° C. or lower, and/or a filtration treatment step. なやし処理工程は、密閉容器へ格納し容器ごと撹拌する方法、乳鉢と乳棒を用いて粉砕する方法、及び擂潰機を用いて撹拌及び粉砕する方法の少なくともいずれかによって行う、請求項8に記載の方法。 Claim 8, wherein the coaxing step is carried out by at least one of the following methods: storing in a closed container and stirring the whole container, pulverizing using a mortar and pestle, and stirring and pulverizing using a crusher. The method described in.
JP2023073090A 2022-04-28 2023-04-27 Method for producing colorful black lacquer Pending JP2023164367A (en)

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